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Method Development and Validation in Food and Pharmaceutical Analysis

A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (31 December 2019) | Viewed by 139880

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Special Issue Editors


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Guest Editor
Department of Manufacturing Pharmacy, College of Pharmacy and Research Institute for Drug Development, Pusan National University, Geumjeong-gu, Busan 46241, Republic of Korea
Interests: bioanalysis; biopharmaceutics; DMPK; PBPK/PD modeling
Special Issues, Collections and Topics in MDPI journals

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Guest Editor
College of Pharmacy, Kangwon National University, Chuncheon 24341, Republic of Korea
Interests: spectroscopy; imaging analysis; formulation; drug delivery system
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Collegues,

Analytical chemistry is the study of separation, identification, and quantification of natural and artificial materials constituting one or more compounds or elements. Rapid growth in food and pharmaceutical industries and production of drugs and functional foods around the world has given rise to an inevitable demand to seek novel and systematic analytical techniques. As a consequence, analytical method development and validation have become a crucial prerequisite for achieving reliable analytical data required to support food and pharmaceutical development processes.

This Special Issue on “Method Development and Validation in Food and Pharmaceutical Analysis” will cover a wide range of topics including, but not limited to, new analytical and bioanalytical methods relevant to the separation, identification, and determination of substances in pharmaceutics, pharmacokinetics, nanobiotechnology, clinical chemistry, and related disciplines; methods for the identification of bioactive compounds in functional foods and medicinal plants; applications of chromatography and allied techniques in biomedical sciences.

We warmly invite our colleagues to submit their original contributions to this Special Issue in order to provide recent updates regarding analytical methods for drugs, biologics, phytochemicals, and other organic/inorganic materials related to food and pharmaceutical sciences that will be of interest to our readers. We would be delighted if you could respond to confirm your contribution and the proposed title by 30 September 2019 to assist in planning the whole project.

Prof. Dr. In-Soo Yoon
Prof. Dr. Hyun-Jong Cho
Guest Editors

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Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Molecules is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2700 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • HPLC
  • bioanalysis
  • phytochemicals
  • pharmacokinetics
  • mass spectrometry
  • functional food
  • biopharmaceutics
  • organic/inorganic materials
  • imaging analysis
  • spectroscopy

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Published Papers (23 papers)

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Research

12 pages, 807 KiB  
Article
Development and Validation of Analytical Method for SH-1242 in the Rat and Mouse Plasma by Liquid Chromatography/Tandem Mass Spectrometry
by Yoo-Seong Jeong, Minjeong Baek, Seungbeom Lee, Min-Soo Kim, Han-Joo Maeng, Jong-Hwa Lee, Young-Ger Suh and Suk-Jae Chung
Molecules 2020, 25(3), 531; https://doi.org/10.3390/molecules25030531 - 25 Jan 2020
Cited by 1 | Viewed by 2838
Abstract
SH-1242, a novel inhibitor of heat shock protein 90 (HSP90), is a synthetic analog of deguelin: It was previously reported that the treatment of SH-1242 led to a strong suppression of hypoxia-mediated retinal neovascularization and vascular leakage in diabetic retinas by inhibiting the [...] Read more.
SH-1242, a novel inhibitor of heat shock protein 90 (HSP90), is a synthetic analog of deguelin: It was previously reported that the treatment of SH-1242 led to a strong suppression of hypoxia-mediated retinal neovascularization and vascular leakage in diabetic retinas by inhibiting the hypoxia-induced upregulation of expression in hypoxia-inducible factor 1α (HIF-1α) and vascular endothelial growth factor (VEGF). In this study, an analytical method for the quantification of SH-1242 in biological samples from rats and mice was developed/validated for application in pharmacokinetic studies. SH-1242 and deguelin, an internal standard of the assay, in plasma samples from the rodents were extracted with methanol containing 0.1% formic acid and analyzed at m/z transition values of 368.9→151.0 and 395.0→213.0, respectively. The method was validated in terms of accuracy, precision, dilution, matrix effects, recovery, and stability and shown to comply with validation guidelines when it was used in the concentration ranges of 1–1000 ng/mL for rat plasma and of 2–1000 ng/mL for mouse plasma. SH-1242 levels in plasma samples were readily determined using the developed method for up to 480 min after the intravenous administration of 0.1 mg/kg SH-1242 to rats and for up to 120 min to mice. These findings suggested that the current method was practical and reliable for pharmacokinetic studies on SH-1242 in preclinical animal species. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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20 pages, 2693 KiB  
Article
Pharmacokinetic Comparison of Epinastine Using Developed Human Plasma Assays
by Seung-Hyun Jeong, Ji-Hun Jang, Hea-Young Cho and Yong-Bok Lee
Molecules 2020, 25(1), 209; https://doi.org/10.3390/molecules25010209 - 03 Jan 2020
Cited by 3 | Viewed by 3719
Abstract
The purpose of the study was to develop two new methods, HPLC-UV and UPLC-MS/MS, for quantifying epinastine in human plasma and to compare pharmacokinetic (PK) parameters obtained using them. Even in the same sample, there may be a difference in the quantitative value [...] Read more.
The purpose of the study was to develop two new methods, HPLC-UV and UPLC-MS/MS, for quantifying epinastine in human plasma and to compare pharmacokinetic (PK) parameters obtained using them. Even in the same sample, there may be a difference in the quantitative value of drug depending on the assay, so that minor changes in PK parameter values may affect drug dose and usage settings. Therefore, selection and establishment of analytical methods are very important in PK studies of drugs, and a comparison of PK parameters according to analytical methods will be vital. For this study of PK parameter change, we newly developed two methods, HPLC-UV and UPLC-MS/MS, which are most commonly used to quantify epinastine concentrations in human plasma. All developed methods satisfied the international guidelines and criteria for successful application to PK study of 20 mg epinastine hydrochloride tablets after oral administration to twenty-six humans. A comparison of these two methods for in vivo analysis of epinastine was performed for the first time. This comparison study confirmed that different dose and usage settings might be possible based on PK parameters calculated using other analyses. Such changes in calculated PK parameters according to analytical methods would be crucial in the clinic. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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15 pages, 1692 KiB  
Article
Development of an Oriental Medicine Discrimination Method through Analysis of Steroidal Saponins in Dioscorea nipponica Makino and Their Anti-Osteosarcoma Effects
by Joo Tae Hwang, Ki-Sun Park, Jin Ah Ryuk, Hye Jin Kim and Byoung Seob Ko
Molecules 2019, 24(22), 4022; https://doi.org/10.3390/molecules24224022 - 06 Nov 2019
Cited by 13 | Viewed by 2986
Abstract
To prevent confusing Dioscorea nipponica (DN), an Oriental medicine, with Dioscorea quinquelobata (DQ) and Dioscorea septemloba (DS), a simple and accurate quantitative analysis method using HPLC combined with ultraviolet (UV) detection was developed and verified with UPLC-QTOF/MS through identification of five saponin glycosides: [...] Read more.
To prevent confusing Dioscorea nipponica (DN), an Oriental medicine, with Dioscorea quinquelobata (DQ) and Dioscorea septemloba (DS), a simple and accurate quantitative analysis method using HPLC combined with ultraviolet (UV) detection was developed and verified with UPLC-QTOF/MS through identification of five saponin glycosides: protodioscin (1), protogracillin (2), pseudoprotodioscin (3), dioscin (4), and gracillin (5). The newly developed analysis method showed sufficient reproducibility (<1.91%) and accuracy (92.1%–102.6%) and was able to identify DN based on the presence of compound 3 (13.821 ± 0.037 mg/mL) and the absence of 5. Compound 1, which is present in DN at a relatively high level (159.983 ± 0.064 mg/mL), was also an important marker for identification. Among the three species, DN showed the strongest activation of apoptotic signaling in osteosarcoma cells, while the four compounds detected in DN showed IC50 values of 6.43 (1), 10.61 (2), 10.48 (3), and 6.90 (4). In conclusion, the strong inhibitory effect of DN against osteosarcoma was confirmed to be associated with 1 and 4, which is also related to the quantitative results. Therefore, the results of this study might provide important information for quality control related to Oriental medicine. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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9 pages, 1948 KiB  
Communication
Validation of a Cell Proliferation Assay to Assess the Potency of a Dialyzable Leukocyte Extract Intended for Batch Release
by Gregorio Carballo-Uicab, José E. Linares-Trejo, Gabriela Mellado-Sánchez, Carlos A. López-Morales, Marco Velasco-Velázquez, Lenin Pavón, Sergio Estrada-Parra, Sonia Mayra Pérez-Tapia and Emilio Medina-Rivero
Molecules 2019, 24(19), 3426; https://doi.org/10.3390/molecules24193426 - 20 Sep 2019
Cited by 3 | Viewed by 5139
Abstract
Transferon® is a blood product with immunomodulatory properties constituted by a complex mixture of peptides obtained from a human dialyzable leukocyte extract (DLE). Due to its complex nature, it is necessary to demonstrate batch consistency in its biological activity. Potency is the [...] Read more.
Transferon® is a blood product with immunomodulatory properties constituted by a complex mixture of peptides obtained from a human dialyzable leukocyte extract (DLE). Due to its complex nature, it is necessary to demonstrate batch consistency in its biological activity. Potency is the quantitative measure of biological activity and is also a quality attribute of drugs. Here we developed and validated a proliferation assay using Jurkat cells exposed to azathioprine, which is intended to determine the potency of Transferon® according to international guidelines for pharmaceuticals. The assay showed a linear response (2.5 to 40 µg/mL), coefficients of variation from 0.7 to 13.6% demonstrated that the method is precise, while r2 = 0.97 between the nominal and measured values obtained from dilutional linearity showed that the method is accurate. We also demonstrated that the cell proliferation response was specific for Transferon® and was not induced by its vehicle nor by other peptide complex mixtures (glatiramer acetate or hydrolyzed collagen). The bioassay validated here was used to assess the relative potency of eight released batches of Transferon® with respect to a reference standard, showing consistent results. The collective information from the validation and the assessment of several batches indicate that the bioassay is suitable for the release of Transferon®. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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9 pages, 1524 KiB  
Communication
Tyrosinase Inhibition Antioxidant Effect and Cytotoxicity Studies of the Extracts of Cudrania tricuspidata Fruit Standardized in Chlorogenic Acid
by Ha-Na Oh, Dae-Hun Park, Ji-Yeon Park, Seung-Yub Song, Sung-Ho Lee, Goo Yoon, Hong-Seop Moon, Deuk-Sil Oh, Sang-Hoon Rhee, Eun-Ok Im, In-Soo Yoon, Jung-Hyun Shim and Seung-Sik Cho
Molecules 2019, 24(18), 3266; https://doi.org/10.3390/molecules24183266 - 07 Sep 2019
Cited by 14 | Viewed by 3247
Abstract
In the present study, various extracts of C. tricuspidata fruit were prepared with varying ethanol contents and evaluated for their biomarker and biological properties. The 80% ethanolic extract showed the best tyrosinase inhibitory activity, while the 100% ethanolic extract showed the best [...] Read more.
In the present study, various extracts of C. tricuspidata fruit were prepared with varying ethanol contents and evaluated for their biomarker and biological properties. The 80% ethanolic extract showed the best tyrosinase inhibitory activity, while the 100% ethanolic extract showed the best total phenolics and flavonoids contents. The HPLC method was applied to analyze the chlorogenic acid in C. tricuspidata fruit extracts. The results suggest that the observed antioxidant and tyrosinase inhibitory activity of C. tricuspidata fruit extract could partially be attributed to the presence of marker compounds in the extract. In this study, we present an analytical method for standardization and optimization of C. tricuspidata fruit preparations. Further investigations are warranted to confirm the in vivo pharmacological activity of C. tricuspidata fruit extract and its active constituents and assess the safe use of the plant for the potential development of the extract as a skin depigmentation agent. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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11 pages, 1178 KiB  
Article
Simultaneous Quantification of Four Phenylethanoid Glycosides in Rat Plasma by UPLC-MS/MS and Its Application to a Pharmacokinetic Study of Acanthus Ilicifolius Herb
by Mengqi Zhang, Xia Ren, Shijun Yue, Qing Zhao, Changlun Shao and Changyun Wang
Molecules 2019, 24(17), 3117; https://doi.org/10.3390/molecules24173117 - 28 Aug 2019
Cited by 9 | Viewed by 2644
Abstract
Acanthus ilicifolius herb (AIH), the dry plant of Acanthus ilicifolius L., has long been used as a folk medicine for treating acute and chronic hepatitis. Phenylethanoid glycosides (PhGs) are one family of the main components in AIH with hepatoprotective, antioxidant, and anti-inflammatory activities. [...] Read more.
Acanthus ilicifolius herb (AIH), the dry plant of Acanthus ilicifolius L., has long been used as a folk medicine for treating acute and chronic hepatitis. Phenylethanoid glycosides (PhGs) are one family of the main components in AIH with hepatoprotective, antioxidant, and anti-inflammatory activities. In this study, the pharmacokinetics of AIH was investigated preliminarily by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-MS/MS). A simultaneously quantitative determination method for four PhGs (acteoside, isoacteoside, martynoside, and crenatoside) in rat plasma was first established by UPLC-MS/MS. These four PhGs were separated with an ACQUITY UPLC BEH C18 column (2.1 × 50 mm, 1.7 μm) by gradient elution (mobile phase: MeCN and 0.1% formic acid in water, 0.4 mL/min). The mass spectrometry detection was performed using negative electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode. By the established method, the preliminary pharmacokinetics of AIH was elucidated using the kinetic parameters of the four PhGs in rat plasma after intragastric administration of AIH ethanol extract. All four PhGs showed double peaks on concentration-time curves, approximately at 0.5 h and 6 h, respectively. Their elimination half-lives (t1/2) were different, ranging from 3.42 h to 8.99 h, although they shared similar molecular structures. This work may provide a basis for the elucidation of the pharmacokinetic characteristics of bioactive components from AIH. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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17 pages, 1746 KiB  
Article
Detection of 13 Ginsenosides (Rb1, Rb2, Rc, Rd, Re, Rf, Rg1, Rg3, Rh2, F1, Compound K, 20(S)-Protopanaxadiol, and 20(S)-Protopanaxatriol) in Human Plasma and Application of the Analytical Method to Human Pharmacokinetic Studies Following Two Week-Repeated Administration of Red Ginseng Extract
by Sojeong Jin, Ji-Hyeon Jeon, Sowon Lee, Woo Youl Kang, Sook Jin Seong, Young-Ran Yoon, Min-Koo Choi and Im-Sook Song
Molecules 2019, 24(14), 2618; https://doi.org/10.3390/molecules24142618 - 18 Jul 2019
Cited by 57 | Viewed by 5630
Abstract
We aimed to develop a sensitive method for detecting 13 ginsenosides using liquid chromatography–tandem mass spectrometry and to apply this method to pharmacokinetic studies in human following repeated oral administration of red ginseng extract. The chromatograms of Rb1, Rb2, Rc, Rd, Re, Rf, [...] Read more.
We aimed to develop a sensitive method for detecting 13 ginsenosides using liquid chromatography–tandem mass spectrometry and to apply this method to pharmacokinetic studies in human following repeated oral administration of red ginseng extract. The chromatograms of Rb1, Rb2, Rc, Rd, Re, Rf, Rg1, Rg3, Rh2, F1, compound K (CK), protopanaxadiol (PPD), and protopanaxatriol (PPT) in human plasma were well separated. The calibration curve range for 13 ginsenosides was 0.5–200 ng/mL and the lower limit of quantitation was 0.5 ng/mL for all ginsenosides. The inter- and intra-day accuracy, precision, and stability were less than 15%. Among the 13 ginsenosides tested, nine ginsenosides (Rb1, Rb2, Rc, Rd, Rg3, CK, Rh2, PPD, and PPT) were detected in the human plasma samples. The plasma concentrations of Rb1, Rb2, Rc, Rd, and Rg3 were correlated with the content in red ginseng extract; however, CK, Rh2, PPD, and PPT were detected although they are not present in red ginseng extract, suggesting the formation of these ginsenosides through the human metabolism. In conclusion, our analytical method could be effectively used to evaluate pharmacokinetic properties of ginsenosides, which would be useful for establishing the pharmacokinetic–pharmacodymic relationship of ginsenosides as well as ginsenoside metabolism in humans. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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8 pages, 780 KiB  
Communication
A Simple HPLC Method for the Quantitative Determination of Silybin in Rat Plasma: Application to a Comparative Pharmacokinetic Study on Commercial Silymarin Products
by Eun-Sol Ha, Dong-Gyun Han, Seong-Wook Seo, Ji-Min Kim, Seon-Kwang Lee, Woo-Yong Sim, In-Soo Yoon and Min-Soo Kim
Molecules 2019, 24(11), 2180; https://doi.org/10.3390/molecules24112180 - 10 Jun 2019
Cited by 10 | Viewed by 3550
Abstract
Silybin (SBN) is a major active constituent of silymarin, a mixture of flavonoids found in fruits and seeds of milk thistle. The aim of this study was to describe a simple bioanalytical method for quantifying SBN in rat plasma. A simple protein deproteinization [...] Read more.
Silybin (SBN) is a major active constituent of silymarin, a mixture of flavonoids found in fruits and seeds of milk thistle. The aim of this study was to describe a simple bioanalytical method for quantifying SBN in rat plasma. A simple protein deproteinization procedure with acetonitrile (ACN) was employed for plasma sample preparation. A reversed column and gradient elution of a mobile phase (mixture of phosphate buffer (pH 5.0) and ACN) were used for chromatographic separation. The selectivity, linearity (50–5000 ng/mL), precision, accuracy, recovery, matrix effect, and stability for this method were validated as per the current Food and Drug Administration (FDA) guidelines. Our method for SBN was applied to a comparative pharmacokinetic study on four different commercial silymarin products. This in vivo rat study demonstrated that product #4 significantly enhanced the relative oral bioavailability of SBN, as compared to product #1–3. Therefore, the bioanalytical method proposed herein could serve as a promising alternative for preclinical pharmacokinetic studies on silymarin products and, by extension, clinical use after partial modification and validation. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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12 pages, 1267 KiB  
Article
Liquid Chromatography-Tandem Mass Spectrometry of Desoxo-Narchinol a and Its Pharmacokinetics and Oral Bioavailability in Rats and Mice
by Subindra Kazi Thapa, Mahesh Upadhyay, Tae Hwan Kim, Soyoung Shin, Sung-Joo Park and Beom Soo Shin
Molecules 2019, 24(11), 2037; https://doi.org/10.3390/molecules24112037 - 28 May 2019
Cited by 4 | Viewed by 4497
Abstract
Desoxo-narchinol A is one of the major active constituents from Nardostachys jatamansi, which has been reported to possess various pharmacological activities, including anti-inflammatory, antioxidant, and anticonvulsant activity. A simple and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for [...] Read more.
Desoxo-narchinol A is one of the major active constituents from Nardostachys jatamansi, which has been reported to possess various pharmacological activities, including anti-inflammatory, antioxidant, and anticonvulsant activity. A simple and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantification of desoxo-narchinol A in two different biological matrices, i.e., rat plasma and mouse plasma, using sildenafil as an internal standard (IS). The method involved simple protein precipitation with acetonitrile and the analyte was separated by gradient elution using 100% acetonitrile and 0.1% formic acid in water as a mobile phase. The MS detection was performed with a turbo electrospray in positive ion mode. The lower limit of quantification was 10 ng/mL in both rat and mouse plasma. Intra- and inter-day accuracies were in the ranges of 97.23–104.54% in the rat plasma and 95.90–110.11% in the mouse plasma. The precisions were within 8.65% and 6.46% in the rat and mouse plasma, respectively. The method was applied to examine the pharmacokinetics of desoxo-narchinol A, and the oral bioavailability of desoxo-narchinol A was 18.1% in rats and 28.4% in mice. The present results may be useful for further preclinical and clinical studies of desoxo-narchinol A. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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14 pages, 2250 KiB  
Article
Simultaneous Determination and Pharmacokinetic Characterization of Glycyrrhizin, Isoliquiritigenin, Liquiritigenin, and Liquiritin in Rat Plasma Following Oral Administration of Glycyrrhizae Radix Extract
by You Jin Han, Bitna Kang, Eun-Ju Yang, Min-Koo Choi and Im-Sook Song
Molecules 2019, 24(9), 1816; https://doi.org/10.3390/molecules24091816 - 10 May 2019
Cited by 34 | Viewed by 4564
Abstract
Glycyrrhizae Radix is widely used as herbal medicine and is effective against inflammation, various cancers, and digestive disorders. We aimed to develop a sensitive and simultaneous analytical method for detecting glycyrrhizin, isoliquiritigenin, liquiritigenin, and liquiritin, the four marker components of Glycyrrhizae Radix extract [...] Read more.
Glycyrrhizae Radix is widely used as herbal medicine and is effective against inflammation, various cancers, and digestive disorders. We aimed to develop a sensitive and simultaneous analytical method for detecting glycyrrhizin, isoliquiritigenin, liquiritigenin, and liquiritin, the four marker components of Glycyrrhizae Radix extract (GRE), in rat plasma using liquid chromatography-tandem mass spectrometry and to apply this analytical method to pharmacokinetic studies. Retention times for glycyrrhizin, isoliquiritigenin, liquiritigenin, and liquiritin were 7.8 min, 4.1 min, 3.1 min, and 2.0 min, respectively, suggesting that the four analytes were well separated without any interfering peaks around the peak elution time. The lower limit of quantitation was 2 ng/mL for glycyrrhizin and 0.2 ng/mL for isoliquiritigenin, liquiritigenin, and liquiritin; the inter- and intra-day accuracy, precision, and stability were less than 15%. Plasma concentrations of glycyrrhizin, isoliquiritigenin, liquiritigenin, and liquiritin were quantified for 24 h after a single oral administration of 1 g/kg GRE to four rats. Among the four components, plasma concentration of glycyrrhizin was the highest and exhibited a long half-life (23.1 ± 15.5 h). Interestingly, plasma concentrations of isoliquiritigenin and liquiritigenin were restored to the initial concentration at 4–10 h after the GRE administration, as evidenced by liquiritin biotransformation into isoliquiritigenin and liquiritigenin, catalyzed by fecal lysate and gut wall enzymes. In conclusion, our analytical method developed for detecting glycyrrhizin, isoliquiritigenin, liquiritigenin, and liquiritin could be successfully applied to investigate their pharmacokinetic properties in rats and would be useful for conducting further studies on the efficacy, toxicity, and biopharmaceutics of GREs and their marker components. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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13 pages, 2309 KiB  
Article
Identification and Determination of Seven Phenolic Acids in Brazilian Green Propolis by UPLC-ESI-QTOF-MS and HPLC
by Shengwei Sun, Meijuan Liu, Jian He, Kunping Li, Xuguang Zhang and Guangling Yin
Molecules 2019, 24(9), 1791; https://doi.org/10.3390/molecules24091791 - 09 May 2019
Cited by 27 | Viewed by 4516
Abstract
Brazilian green propolis is a complex mixture of natural compounds that is difficult to analyze and standardize; as a result, controlling its quality is challenging. In this study, we used the positive and negative modes of ultra-performance liquid chromatography coupled with electrospray ionization [...] Read more.
Brazilian green propolis is a complex mixture of natural compounds that is difficult to analyze and standardize; as a result, controlling its quality is challenging. In this study, we used the positive and negative modes of ultra-performance liquid chromatography coupled with electrospray ionization quadrupole time of flight mass spectrometry in conjunction with high-performance liquid chromatography for the identification and characterization of seven phenolic acid compounds in Brazilian green propolis. The optimal operating conditions for the electrospray ionization source were capillary voltage of 3500 V and drying and sheath gas temperatures of 320 °C and 350 °C, respectively. Drying and sheath gas flows were set to 8 L/min and 11 L/min, respectively. Brazilian green propolis was separated using the HPLC method, with chromatograms for samples and standards measured at 310 nm. UPLC-ESI-QTOF-MS was used to identify the following phenolic compounds: Chlorogenic acid, caffeic acid, isochlorogenic acid A, isochlorogenic acid B, isochlorogenic acid C, caffeic acid phenethyl ester (CAPE), and artepillin C. Using a methodologically validated HPLC method, the seven identified phenolic acids were then quantified among different Brazilian green propolis. Results indicated that there were no significant differences in the content of a given phenolic acid across different Brazilian green propolis samples, owing to the same plant resin sources for each sample. Isochlorogenic acid B had the lowest content (0.08 ± 0.04) across all tested Brazilian green propolis samples, while the artepillin C levels were the highest (2.48 ± 0.94). The total phenolic acid content across Brazilian green propolis samples ranged from 2.14–9.32%. Notably, artepillin C quantification is an important factor in determining the quality index of Brazilian green propolis; importantly, it has potential as a chemical marker for the development of better quality control methods for Brazilian green propolis. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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14 pages, 1243 KiB  
Article
Quantification of Furosine (Nε-(2-Furoylmethyl)-l-lysine) in Different Parts of Velvet Antler with Various Processing Methods and Factors Affecting Its Formation
by Rui-ze Gong, Yan-hua Wang, Kun Gao, Lei Zhang, Chang Liu, Ze-shuai Wang, Yu-fang Wang and Yin-shi Sun
Molecules 2019, 24(7), 1255; https://doi.org/10.3390/molecules24071255 - 31 Mar 2019
Cited by 6 | Viewed by 3350
Abstract
Furosine (Nε-(2-furoylmethyl)-l-lysine) is formed during the early stages of the Maillard reaction from a lysine Amadori compound and is frequently used as a marker of reaction progress. Furosine is toxic, with significant effects on animal livers, kidneys, and other [...] Read more.
Furosine (Nε-(2-furoylmethyl)-l-lysine) is formed during the early stages of the Maillard reaction from a lysine Amadori compound and is frequently used as a marker of reaction progress. Furosine is toxic, with significant effects on animal livers, kidneys, and other organs. However, reports on the formation of furosine in processed velvet antler are scarce. In this study, we have quantified the furosine content in processed velvet antler by using UPLC-MS/MS. The furosine contents of velvet antler after freeze-drying, boiling, and processing without and with blood were 148.51–193.93, 168.10–241.22, 60.29–80.33, and 115.18–138.99 mg/kg protein, respectively. The factors affecting furosine formation in processed velvet antler, including reducing sugars, proteins, amino acids, and process temperature, are discussed herein. Proteins, amino acids, and reducing sugars are substrates for the Maillard reaction and most significantly influence the furosine content in the processed velvet antler. High temperatures induce the production of furosine in boiled velvet antler but not in the freeze-dried samples, whereas more furosine is produced in velvet antler processed with blood, which is rich in proteins, amino acids, and reducing sugars, than in the samples processed without blood. Finally, wax slices rich in proteins, amino acids, and reducing sugars produced more furosine than the other parts of the velvet antler. These data provide a reference for guiding the production of low-furosine velvet antler and can be used to estimate the consumer intake of furosine from processed velvet antler. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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16 pages, 1116 KiB  
Article
Two Approaches for Evaluating the Effects of Galangin on the Activities and mRNA Expression of Seven CYP450
by Yin-Ling Ma, Feng Zhao, Jin-Tuo Yin, Cai-Juan Liang, Xiao-Li Niu, Zhi-Hong Qiu and Lan-Tong Zhang
Molecules 2019, 24(6), 1171; https://doi.org/10.3390/molecules24061171 - 25 Mar 2019
Cited by 18 | Viewed by 3537
Abstract
Galangin is a marker compound of honey and Alpinia officinarum Hance that exhibits great potential for anti-microbial, anti-diabetic, anti-obesity, anti-tumour and anti-inflammatory applications. Galangin is frequently consumed in combination with common clinical drugs. Here, we evaluated the effects of galangin on cytochrome P450 [...] Read more.
Galangin is a marker compound of honey and Alpinia officinarum Hance that exhibits great potential for anti-microbial, anti-diabetic, anti-obesity, anti-tumour and anti-inflammatory applications. Galangin is frequently consumed in combination with common clinical drugs. Here, we evaluated the effects of galangin on cytochrome P450 (CYP)-mediated metabolism, using two different approaches, to predict drug–drug interactions. Male Sprague Dawley rats were administered galangin daily for 8 weeks. A “cocktail-probes” approach was employed to evaluate the activities of different CYP450 enzymes. Blood samples of seven probe drugs were analysed using liquid chromatography-tandem mass spectrometry in positive and negative electrospray-ionisation modes. Pharmacokinetic parameters were calculated to identify statistical differences. CYP mRNA-expression levels were investigated in real-time quantitative polymerase chain reaction experiments. The galangin-treated group showed significantly decreased AUC0–∞ and Cmax values for CYP1A2, and CYP2B3. The galangin-treated group showed significantly increased AUC0–∞ and Cmax values for CYP2C13 and CYP3A1. No significant influences were observed in the pharmacokinetic profiles of CYP2C11, CYP2D4 and CYP2E1. The mRNA-expression results were consistent with the pharmacokinetic results. Thus, CYP450 enzyme activities may be altered by long-term galangin administration, suggesting galangin to be a promising candidate molecule for enhancing oral drug bioavailability and chemoprevention and reversing multidrug resistance. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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13 pages, 1740 KiB  
Article
Bioactivity Determination of a Therapeutic Recombinant Human Keratinocyte Growth Factor by a Validated Cell-based Bioassay
by Wenrong Yao, Ying Guo, Xi Qin, Lei Yu, Xinchang Shi, Lan Liu, Yong Zhou, Jinpan Hu, Chunming Rao and Junzhi Wang
Molecules 2019, 24(4), 699; https://doi.org/10.3390/molecules24040699 - 15 Feb 2019
Cited by 5 | Viewed by 3668
Abstract
The therapeutic recombinant human keratinocyte growth factor 1 (rhKGF-1) was approved by the FDA for oral mucositis resulting from hematopoietic stem cell transplantation for hematological malignancies in 2004. However, no recommended bioassay for rhKGF-1 bioactivity has been recorded in the U.S. Pharmacopoeia. In [...] Read more.
The therapeutic recombinant human keratinocyte growth factor 1 (rhKGF-1) was approved by the FDA for oral mucositis resulting from hematopoietic stem cell transplantation for hematological malignancies in 2004. However, no recommended bioassay for rhKGF-1 bioactivity has been recorded in the U.S. Pharmacopoeia. In this study, we developed an rhKGF-1-dependent bioassay for determining rhKGF-1 bioactivity based on HEK293 and HaCat cell lines that stably expressed the luciferase reporter driven by the serum response element (SRE) and human fibroblast growth factor receptor (FGFR2) IIIb. A good responsiveness to rhKGF-1 and rhKGF-2 shared by target HEK293/HaCat cell lines was demonstrated. Our stringent validation was completely focused on specificity, linearity, accuracy, precision, and robustness according to the International Council for Harmonization (ICH) Q2 (R1) guidelines, AAPS/FDA Bioanalytical Workshop and the Chinese Pharmacopoeia. We confirmed the reliability of the method in determining rhKGF bioactivity. The validated method is highly timesaving, sensitive, and simple, and is especially valuable for providing information for quality control during the manufacture, research, and development of therapeutic rhKGF. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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10 pages, 779 KiB  
Article
Identification and Extraction Optimization of Active Constituents in Citrus junos Seib ex TANAKA Peel and Its Biological Evaluation
by Jung-hyun Shim, Jung-il Chae and Seung-sik Cho
Molecules 2019, 24(4), 680; https://doi.org/10.3390/molecules24040680 - 14 Feb 2019
Cited by 14 | Viewed by 2785
Abstract
Citrus junos Seib ex TANAKA possesses various biological effects. It has been used in oriental remedies for blood circulation and the common cold. Recently, biological effects of C. junos peel have been reported. However, optimization of the biological properties of C. junos peel [...] Read more.
Citrus junos Seib ex TANAKA possesses various biological effects. It has been used in oriental remedies for blood circulation and the common cold. Recently, biological effects of C. junos peel have been reported. However, optimization of the biological properties of C. junos peel preparations has yet to be reported on. We developed a high-performance liquid chromatography (HPLC) method for quantification of the active constituents in C. junos peel. Hot water and ethanolic extracts of C. junos peel were prepared and their chemical profiles and biological activities were evaluated. The 80% ethanolic extract demonstrated the greatest antioxidant activity and phenolic content, while the 100% ethanolic extract had the greatest xanthine oxidase inhibitory activity. Elastase inhibition activity was superior in aqueous and 20% ethanolic extracts. The contents of two flavonoids were highest in the 100% ethanolic extract. We postulated that the antioxidant and anti-aging effects of C. junos peel extract could be attributed to phenolics such as flavonoids. Our results suggest that the flavonoid-rich extract of C. junos may be utilized for the treatment and prevention of metabolic disease and hyperuricemia while the water-soluble extract of C. junos could be used as a source for its anti-aging properties. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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8 pages, 1282 KiB  
Communication
Phytochemical Constituents and the Evaluation Biological Effect of Cinnamomum yabunikkei H.Ohba Leaf
by Seung-Yub Song, Seung-Hui Song, Min-Suk Bae and Seung-Sik Cho
Molecules 2019, 24(1), 81; https://doi.org/10.3390/molecules24010081 - 27 Dec 2018
Cited by 3 | Viewed by 2680
Abstract
Cinnamomum yabunikkei H.Ohba leaf is known as a traditional medicinal material in Korea. However, no scientific identification of the components or efficacy of C.yabunikkei H.Ohba leaf has been reported. In the present study, we prepared various solvent extracts of C.yabunikkei H.Ohba leaf to [...] Read more.
Cinnamomum yabunikkei H.Ohba leaf is known as a traditional medicinal material in Korea. However, no scientific identification of the components or efficacy of C.yabunikkei H.Ohba leaf has been reported. In the present study, we prepared various solvent extracts of C.yabunikkei H.Ohba leaf to understand its basic properties and evaluated the antioxidant, xanthine oxidase inhibitory, and elastase inhibitory activities of hexane, ethyl acetate, acetone, methanol, ethanol, and water extracts for the first time. The antioxidant properties were evaluated based on 1,1-diphenyl-2-picrylhydrazyl (DPPH) free radical scavenging activity, reducing power, and total phenolic contents. The hot water extract showed the highest DPPH radical scavenging activity and total phenolic contents, and the reducing power was the highest in the water extract. The hexane extract showed an excellent elastase inhibitory effect compared to control (phosphoramidone) and the highest xanthine oxidase inhibitory activity. These results present basic information for the possible uses of the hot water and hexane extracts from C. yabunikkei leaf for the treatment of diseases caused by oxidative imbalance. In the present study, individual extracts exhibited different effects. Therefore, it is hypothesized that the applicability of C. yabunikkei will depend on the extraction method and nature of the extract. The hot water and hexane extracts could be used as antioxidants, and as anti-gout and anti-wrinkle materials respectively. Several biologically active substances present in hexane extract of C. yabunikkei have been analyzed by GCMS and demonstrated to possess antioxidant and xanthine oxidase inhibitory activity. To the best of our knowledge, this is the first study that reports the chemical profiling and biological effects of various C. yabunikkei leaf extracts, suggesting their potential use in food therapy, cosmetics or alternative medicine. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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13 pages, 658 KiB  
Article
Simultaneous Determination of Nε-(carboxymethyl) Lysine and Nε-(carboxyethyl) Lysine in Different Sections of Antler Velvet after Various Processing Methods by UPLC-MS/MS
by Rui-ze Gong, Yan-hua Wang, Yu-fang Wang, Bao Chen, Kun Gao and Yin-shi Sun
Molecules 2018, 23(12), 3316; https://doi.org/10.3390/molecules23123316 - 14 Dec 2018
Cited by 13 | Viewed by 3282
Abstract
Nε-(Carboxymethyl) lysine (CML) and Nε-(carboxyethyl) advanced glycation end-products (AGEs) and are frequently used as markers of AGE formation. AGEs, such as CML and CEL, have harmful effects in the human body and have been closely linked to many diseases [...] Read more.
Nε-(Carboxymethyl) lysine (CML) and Nε-(carboxyethyl) advanced glycation end-products (AGEs) and are frequently used as markers of AGE formation. AGEs, such as CML and CEL, have harmful effects in the human body and have been closely linked to many diseases such as diabetes and uremia. However, details on the contents of CML and CEL after applying different antler velvet processing methods are lacking. In this research, a robust lysine (CEL) are two typical UPLC-MS/MS method has been developed for the simultaneous determination of CML and CEL in various sections of antler velvet processed with different methods. In addition, factors affecting the CML and CEL contents are discussed. The CML contents of antler velvet after freeze-drying, boiling, processing without blood, and processing with blood were 74.55–458.59, 119.44–570.69, 75.36–234.92, and 117.11–456.01 μg/g protein, respectively; the CEL contents were 0.74–12.66, 11.33–35.93, 0.00–6.75, and 0.00–23.41 μg/g protein, respectively. The different contents of CML and CEL in the different samples of antler velvet result from the different interactions of the protein and lysine at different temperatures. These data can be used to estimate the potential consumer intake of CML and CEL from antler velvet and for guiding producers on how to reduce the production of CML and CEL. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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8 pages, 878 KiB  
Communication
Optimization of the Extraction Conditions and Biological Evaluation of Dendropanax morbifera H. Lev as an Anti-Hyperuricemic Source
by Seung-Sik Cho, Seung-Hui Song, Chul-Yung Choi, Kyung Mok Park, Jung-Hyun Shim and Dae-Hun Park
Molecules 2018, 23(12), 3313; https://doi.org/10.3390/molecules23123313 - 14 Dec 2018
Cited by 10 | Viewed by 3012
Abstract
Dendropanax morbifera H. Levis a medicinal plant native to South Korea, East Asia, and South America. Among some 75 species, one species grows in Korea. In previous studies, D. morbifera extracts with anti-oxidant, anti-inflammatory, anti-complementary and anti-cancer activities were reported. The present study [...] Read more.
Dendropanax morbifera H. Levis a medicinal plant native to South Korea, East Asia, and South America. Among some 75 species, one species grows in Korea. In previous studies, D. morbifera extracts with anti-oxidant, anti-inflammatory, anti-complementary and anti-cancer activities were reported. The present study aims to investigate optimization of extraction and evaluation of anti-hyperuricemic effects of D. morbifera leaf and the phytochemicals contained therein. Ethanol and hexane extract were found to display the best xanthine oxidase inhibition among six types of solvent and water extract. The antioxidant effect of the ethanol extract was superior to that of the hexane extract. The DPPH radical scavenging effect of the ethanol and hexane extracts were 81.52 ± 1.57% and 2.69 ± 0.16. The reducing power of the ethanol and hexane extracts were 9.71 ± 0.15 and 0.89 ± 0.01 mg/g equivalent of gallic acid. Total phenols of the ethanol and hexane extracts were 6.53 ± 0.16 and 0.63 ± 0.001 mg/g equivalent of gallic acid. In addition, we compared the two marker compounds from D. morbifera, chlorogenic acid and rutin, which were determined in the ethanol extract at 0.80 ± 0.03% and 0.52 ± 0.01%, respectively. We found that the ethanol extracts showed better xanthine oxidase inhibition than hexane extracts. Especially, ethanol extracts showed higher antioxidant activity than hexane extracts. Based on these results, we selected the ethanol extract as an effective xanthine oxidase inhibitor and confirmed whether ethanol extracts showed xanthine oxidase inhibition in animal experiments. The in vivo mouse study demonstrated that ethanol extract of D. morbifera leaf at the dose of 300 mg/kg could inhibit blood/hepatic xanthine oxidase activity and this result shows that the xanthine oxidase inhibitory activity in vitro is reproduced in vivo. The present study showed that ethanol extract was optimal xanthine oxidase inhibitor which can be applied to prevent diseases related to hyperuricemia. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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15 pages, 2515 KiB  
Article
Identification and Analysis of Compound Profiles of Sinisan Based on ‘Individual Herb, Herb-Pair, Herbal Formula’ before and after Processing Using UHPLC-Q-TOF/MS Coupled with Multiple Statistical Strategy
by Jia Zhou, Hao Cai, Sicong Tu, Yu Duan, Ke Pei, Yangyang Xu, Jing Liu, Minjie Niu, Yating Zhang, Lin Shen and Qigang Zhou
Molecules 2018, 23(12), 3128; https://doi.org/10.3390/molecules23123128 - 29 Nov 2018
Cited by 24 | Viewed by 50680
Abstract
Sinisan has been widely used to treat depression. However, its pharmacologically-effective constituents are largely unknown, and the pharmacological effects and clinical efficacies of Sinisan-containing processed medicinal herbs may change. To address these important issues, we developed an ultra-high performance liquid chromatography coupled with [...] Read more.
Sinisan has been widely used to treat depression. However, its pharmacologically-effective constituents are largely unknown, and the pharmacological effects and clinical efficacies of Sinisan-containing processed medicinal herbs may change. To address these important issues, we developed an ultra-high performance liquid chromatography coupled with electrospray ionization tandem quadrupole-time-of-flight mass spectrometry (UHPLC-Q-TOF/MS) method coupled with multiple statistical strategies to analyze the compound profiles of Sinisan, including individual herb, herb-pair, and complicated Chinese medicinal formula. As a result, 122 different constituents from individual herb, herb-pair, and complicated Chinese medicinal formula were identified totally. Through the comparison of three progressive levels, it suggests that processing herbal medicine and/or altering medicinal formula compatibility could change herbal chemical constituents, resulting in different pharmacological effects. This is also the first report that saikosaponin h/i and saikosaponin g have been identified in Sinisan. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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16 pages, 7966 KiB  
Article
Identification, Characterization and Quantification of Process-Related and Degradation Impurities in Lisdexamfetamine Dimesylate: Identifiction of Two New Compounds
by Shenghua Gao, Lili Meng, Chunjie Zhao, Tao Zhang, Pengcheng Qiu and Fuli Zhang
Molecules 2018, 23(12), 3125; https://doi.org/10.3390/molecules23123125 - 29 Nov 2018
Cited by 2 | Viewed by 5554
Abstract
Twelve impurities (process-related and degradation) in lisdexamfetamine dimesylate (LDX), a central nervous system (CNS) stimulant drug, were first separated and quantified by high-performance liquid chromatography (HPLC) and then identified by liquid chromatography mass spectrometry (LC-MS). The structures of the twelve impurities were further [...] Read more.
Twelve impurities (process-related and degradation) in lisdexamfetamine dimesylate (LDX), a central nervous system (CNS) stimulant drug, were first separated and quantified by high-performance liquid chromatography (HPLC) and then identified by liquid chromatography mass spectrometry (LC-MS). The structures of the twelve impurities were further confirmed and characterized by IR, HRMS and NMR analyses. Based on the characterization data, two previously unknown impurities formed during the process development and forced degradation were proposed to be (2S)-2,6-di-(lysyl)-amino-N-[(1S)-1-methyl-2-phenyl ethyl]hexanamide (Imp-H) and (2S)-2,6-diamino-N-[(1S)-1-methyl-2-(2-hydroxyphenyl)ethyl] hexanamide (Imp-M). Furthermore, these two compounds are new. Probable mechanisms for the formation of the twelve impurities were discussed based on the synthesis route of LDX. Superior separation was achieved on a YMC-Pack ODS-AQ S5 120A silica column (250 × 4.6 mm × 5 μm) using a gradient of a mixture of acetonitrile and 0.1% aqueous methanesulfonic acid solution. The HPLC method was optimized in order to separate, selectively detect, and quantify all the impurities. The full identification and characterization of these impurities should prove useful for quality control in the manufacture of lisdexamfetamine dimesylate. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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19 pages, 1334 KiB  
Article
Derivatization of Methylglyoxal for LC-ESI-MS Analysis—Stability and Relative Sensitivity of Different Derivatives
by Stefan Fritzsche, Susan Billig, Robby Rynek, Ramarao Abburi, Elena Tarakhovskaya, Olga Leuner, Andrej Frolov and Claudia Birkemeyer
Molecules 2018, 23(11), 2994; https://doi.org/10.3390/molecules23112994 - 16 Nov 2018
Cited by 10 | Viewed by 7113
Abstract
The great research interest in the quantification of reactive carbonyl compounds (RCCs), such as methylglyoxal (MGO) in biological and environmental samples, is reflected by the fact that several publications have described specific strategies to perform this task. Thus, many reagents have also been [...] Read more.
The great research interest in the quantification of reactive carbonyl compounds (RCCs), such as methylglyoxal (MGO) in biological and environmental samples, is reflected by the fact that several publications have described specific strategies to perform this task. Thus, many reagents have also been reported for the derivatization of RCCs to effectively detect and quantify the resulting compounds using sensitive techniques such as liquid chromatography coupled with mass spectrometry (LC-MS). However, the choice of the derivatization protocol is not always clear, and a comparative evaluation is not feasible because detection limits from separate reports and determined with different instruments are hardly comparable. Consequently, for a systematic comparison, we tested 21 agents in one experimental setup for derivatization of RCCs prior to LC-MS analysis. This consisted of seven commonly employed reagents and 14 similar reagents, three of which were designed and synthesized by us. All reagents were probed for analytical responsiveness of the derivatives and stability of the reaction mixtures. The results showed that derivatives of 4-methoxyphenylenediamine and 3-methoxyphenylhydrazine—reported here for the first time for derivatization of RCCs—provided a particularly high responsiveness with ESI-MS detection. We applied the protocol to investigate MGO contamination of laboratory water and show successful quantification in a lipoxidation experiment. In summary, our results provide valuable information for scientists in establishing accurate analysis of RCCs. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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10 pages, 1769 KiB  
Article
An Accurate and Effective Method for Measuring Osimertinib by UPLC-TOF-MS and Its Pharmacokinetic Study in Rats
by Song-Tao Dong, Ying Li, Hao-Tian Yang, Yin Wu, Ya-Jing Li, Cong-Yang Ding, Lu Meng, Zhan-Jun Dong and Yuan Zhang
Molecules 2018, 23(11), 2894; https://doi.org/10.3390/molecules23112894 - 06 Nov 2018
Cited by 10 | Viewed by 3645
Abstract
Osimertinib, a new-generation inhibitor of the epidermal growth factor, has been used for the clinical treatment of advanced T790M mutation-positive tumors. In this research, an original analysis method was established for the quantification of osimertinib by ultra-performance liquid chromatography with time of flight [...] Read more.
Osimertinib, a new-generation inhibitor of the epidermal growth factor, has been used for the clinical treatment of advanced T790M mutation-positive tumors. In this research, an original analysis method was established for the quantification of osimertinib by ultra-performance liquid chromatography with time of flight mass spectrometry (UPLC-TOF-MS) in rat plasma. After protein precipitation with acetonitrile and sorafinib (internal standard, IS), they were chromatographed through a Waters XTerra MS C18 column. The mobile phase was acetonitrile and water (including 0.1% ammonia). The relative standard deviation (RSD) of the intra- and inter-day results ranged from 5.38 to 9.76% and from 6.02 to 9.46%, respectively, and the extraction recovery and matrix effects were calculated to range from 84.31 to 96.14% and from 91.46 to 97.18%, respectively. The results illustrated that the analysis method had sufficient specificity, accuracy and precision. Meanwhile, the UPLC-TOF-MS method for osimertinib was successfully applied into the pharmacokinetics of SD rats. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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16 pages, 1190 KiB  
Article
Partial Purification, Identification, and Quantitation of Antioxidants from Wild Rice (Zizania latifolia)
by Mei-Jun Chu, Xin-Min Liu, Ning Yan, Feng-Zhong Wang, Yong-Mei Du and Zhong-Feng Zhang
Molecules 2018, 23(11), 2782; https://doi.org/10.3390/molecules23112782 - 26 Oct 2018
Cited by 27 | Viewed by 4382
Abstract
To provide further insights into the potential health-promoting antioxidants from wild rice (Zizania latifolia), which is an abundant but underutilized whole grain resource in East Asia, a partial purification based on D101 macroporous resin was carried out for the purification and [...] Read more.
To provide further insights into the potential health-promoting antioxidants from wild rice (Zizania latifolia), which is an abundant but underutilized whole grain resource in East Asia, a partial purification based on D101 macroporous resin was carried out for the purification and enrichment of the antioxidants from the bioactive ethanol extracts of wild rice. On that basis, 34 phenolic compounds in the antioxidant fractions were identified by a high-performance liquid chromatography-linear ion trap quadrupole-Orbitrap-mass spectrometry (HPLC-LTQ-Orbitrap-MSn). The results suggested that phenolic acids could be enriched in the 10% ethanol-eluted fraction whereas flavonoids (including procyanidins and flavonoid glycosides) could be enriched in 20–30% ethanol-eluted fractions. A quantitative analysis determined by the multiple reaction monitoring mode of the ultra-performance liquid chromatography-triple quadrupole-tandem mass spectrometry (UPLC-QqQ-MS/MS) revealed a high content of procyanidins in wild rice. Compared with phenolic acids, flavonoids may contribute more to the potent antioxidant activity of wild rice. This is the first study on the antioxidants from wild rice Z. latifolia. These findings provide novel information on the functional components of wild rice, and will be of value to further research and development on Z. latifolia. Full article
(This article belongs to the Special Issue Method Development and Validation in Food and Pharmaceutical Analysis)
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