Research

13 pages, 1370 KiB

Open AccessArticle

Terminal Residue and Dietary Risk Assessment of Atrazine and Isoxaflutole in Corn Using High-Performance Liquid Chromatography–Tandem Mass Spectrometry

by Junli Cao, Tao Pei, Yonghui Wang, Shu Qin, Yanli Qi, Pengcheng Ren and Jindong Li

Molecules 2023, 28(20), 7225; https://doi.org/10.3390/molecules28207225 - 23 Oct 2023

Cited by 1 | Viewed by 888

Abstract

Isoxaflutole and atrazine are representative pesticides for weed control in corn fields. Formulations containing these two pesticides have been registered in China, and their residues may threaten food safety and human health. In this study, a method for simultaneous determination of isoxaflutole, atrazine, [...] Read more.

Isoxaflutole and atrazine are representative pesticides for weed control in corn fields. Formulations containing these two pesticides have been registered in China, and their residues may threaten food safety and human health. In this study, a method for simultaneous determination of isoxaflutole, atrazine, and their metabolites in fresh corn, corn kernels, and corn straw was established based on modified QuEChERS pre-treatment and high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS). The linearity of seven compounds was good (R² ≥ 0.9912), and the matrix effect was 48.5–77.1%. At four spiked levels of 0.01, 0.02, 0.05, and 0.5 mg kg⁻¹, all compounds’ average recovery was 76% to 116%, with relative standard deviation (RSD) less than 18.9%. Field experiments were conducted in Liaoning, Heilongjiang, Inner Mongolia, Shanxi, Beijing, and Yunnan provinces to study the terminal residues. The terminal residues of all compounds were below the LOQ (0.01 mg kg⁻¹) in fresh corn and corn kernels, and atrazine residues in corn straw ranged from <0.05 mg kg⁻¹ to 0.17 mg kg⁻¹. Finally, a dietary risk assessment was conducted based on residues from field trials, food consumption, and acceptable daily intake (ADI). For all populations, the chronic dietary risk probability (RQ_c) of atrazine was between 0.0185% and 0.0739%, while that of isoxaflutole was 0.0074–0.0296%, much lower than 100%. The results may provide scientific guidance for using isoxaflutole and atrazine in corn field ecosystems. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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14 pages, 594 KiB

Open AccessArticle

A Green Bridge: Enhancing a Multi-Pesticide Test for Food by Phase-Transfer Sample Treatment Coupled with LC/MS

by Shaoming Jin, Yi Shen, Tongtong Liu, Ruiqiang Liang, Xiao Ning and Jin Cao

Molecules 2023, 28(19), 6756; https://doi.org/10.3390/molecules28196756 - 22 Sep 2023

Viewed by 722

Abstract

The preparation and treatment of the sample has become an important part of the determination process, which directly affects the accuracy of detection. The preparation of the sample for final detection is actually a process of separation and transfer of the target to [...] Read more.

The preparation and treatment of the sample has become an important part of the determination process, which directly affects the accuracy of detection. The preparation of the sample for final detection is actually a process of separation and transfer of the target to be tested from the sample matrix. The phase-transfer process of analysis and detection is the process of transferring the target substance to be measured from a complex multiphase system to a simple homogeneous system. This study shows a new phase-transfer process for food sample pretreatment in the determination of carbamate pesticides. Edible gum, xanthan gum, carrageenan, and gelatin were selected for purification testing from the perspective of eco-friendliness and safety. Phase-transfer purification process research was carried out on spinach and other foods. Compared with the commonly used QuEChERS method, the LC/MS results indicate that the straightforward carrageenan treatment process can significantly diminish the detection matrix effect and yield similarly superior detection parameters. The phase-transfer purification method with carrageenan has similar sensitivity and systematic error. The limits of detection and limits of quantitation of each pesticide compound in six plant sample substrates were 0.02–0.36 μg/kg and 0.06–1.9 μg/kg, respectively, which were lower than the residue limits here and abroad. Supplemental recoveries in six blank samples at 5, 20, and 100 μg/kg with the phase-transfer process method were better than those for the QuEChERS method. Positive determination results of actual samples using carrageenan phase-transfer purification proved that this method can be used for related detection from a practical point of view. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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11 pages, 1435 KiB

Open AccessArticle

Simultaneous Determination of 54 Pesticides in Proso Millet Using QuEChERS with Liquid Chromatography-Tandem Mass Spectrometry (LC–MS/MS)

by Chao Ding, Pengcheng Ren, Yanli Qi, Yanmei Yang and Shu Qin

Molecules 2023, 28(18), 6575; https://doi.org/10.3390/molecules28186575 - 12 Sep 2023

Viewed by 724

Abstract

To assess the potential risks posed to the environment and human health, analyzing pesticide residues in proso millet is important. This paper aimed to develop a modified QuEChERS method with liquid chromatography-tandem mass spectrometry (LC–MS/MS) for the analysis of 54 pesticide residues in [...] Read more.

To assess the potential risks posed to the environment and human health, analyzing pesticide residues in proso millet is important. This paper aimed to develop a modified QuEChERS method with liquid chromatography-tandem mass spectrometry (LC–MS/MS) for the analysis of 54 pesticide residues in proso millet. Parameters including the mobile phase of the instrument, the acidity of the extraction solvent, and the type of absorbents were optimized to provide satisfactory performance. The method was validated concerning linearity, limit of quantification (LOQ), matrix effect, accuracy, and precision. In detail, the linearity of the matrix-matched calibration curve was acceptable with correlation coefficients (R²) higher than 0.99. The mean recovery was in the range of 86% to 114% with relative standard deviations (RSDs) ≤ 20% (n = 5). The LOQ was determined to be 0.25–10 μg/kg. The developed method was feasible for the determination of multiple pesticide residues in proso millet. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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15 pages, 1865 KiB

Open AccessArticle

Pesticide Residues in Mandarins: Three-Year Monitoring Results

by Emrah Gormez, Ozgur Golge, Miguel Ángel González-Curbelo and Bulent Kabak

Molecules 2023, 28(14), 5611; https://doi.org/10.3390/molecules28145611 - 24 Jul 2023

Cited by 2 | Viewed by 1282

Abstract

The demand of plant production product use has increased because of the current system of citrus production, which prioritizes high agricultural yields. Therefore, the monitoring of pesticide residues in citrus fruits and other agricultural products and their impacts on human health and food [...] Read more.

The demand of plant production product use has increased because of the current system of citrus production, which prioritizes high agricultural yields. Therefore, the monitoring of pesticide residues in citrus fruits and other agricultural products and their impacts on human health and food security are of great concern. This study aims to determine multi-class pesticides including highly polar residues in satsuma mandarins. A total of 226 mandarin samples were collected over three consecutive harvesting years from 2019 to 2021 in the Izmir region of Turkey. Targeted compounds included pesticides and metabolites with European Union (EU) regulatory levels, plus other non-approved residues and highly polar compounds. The residues excluding highly polar substances were analyzed by applying the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction and liquid chromatography–triple quadrupole mass spectrometry (LC-MS/MS) determination for 434 analytes and gas chromatography–triple quadrupole mass spectrometry (GC-MS/MS) determination for 71 analytes. For six highly polar pesticides, sample preparation was based on Quick Polar Pesticides (QuPPe) extraction. The polar residues were determined by LC-MS/MS using internal standards. Forty different residues, including two highly polar substances, were recorded in mandarin samples through three harvesting years. In 8.4% of the samples, no quantifiable residues were detected, whereas 207 samples contained at least one residue. The maximum residue level (MRL) exceedances were recorded for 22.1% of the samples. The two most frequently found pesticides were phosphonic acid and spirotetramat, with an incidence rate of 48.7% and 46.5%, respectively. The concentration of phosphonic acid and spirotetramat in mandarin samples varied from 0.026 to 39.386 mg kg⁻¹ and from 0.010 to 1.485 mg kg⁻¹, respectively. The results will enable researchers and regulatory authorities to assess the extent of pesticide presence, identify potential risks, and take necessary measures to ensure the safety of satsuma mandarins for consumers. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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9 pages, 957 KiB

Open AccessArticle

Chromatographic Method for Monitoring of Pesticide Residues and Risk Assessment for Herbal Decoctions Used in Traditional Korean Medicine Clinics

by Se-Mi Kang, Jae-Hee Won, Ji-Eun Han, Jong-Hyun Kim, Kyeong-Han Kim, Hye-In Jeong and Soo-Hyun Sung

Molecules 2023, 28(8), 3343; https://doi.org/10.3390/molecules28083343 - 10 Apr 2023

Cited by 6 | Viewed by 1276

Abstract

The presence of pesticide residues in herbs and the herbal products derived from them raises serious health concerns. This study was conducted to investigate the residual pesticide concentrations and assess potential human health risks from herbal medicines used in traditional Korean medicine clinics. [...] Read more.

The presence of pesticide residues in herbs and the herbal products derived from them raises serious health concerns. This study was conducted to investigate the residual pesticide concentrations and assess potential human health risks from herbal medicines used in traditional Korean medicine clinics. A total of 40 samples of herbal decoctions were collected from 10 external herbal dispensaries. The pesticide residues were analyzed by the multiresidue method for 320 different pesticides using liquid chromatography tandem mass spectrometry (LC-MS/MS) and gas chromatography tandem mass spectrometry (GC-MS/MS). As a result of the monitoring, carbendazim was detected at 0.01 and 0.03 μg/g in eight samples and no pesticide was detected in the other herbal decoctions. Carbendazim was set for each individual item as less than 0.05 μg/g in Paeoniae radix, less than 0.05 μg/g in Cassiae semen, less than 2.0 μg/g in Lycii fructus, and less than 10 μg/g in Schisandrae fructus (dried). Therefore, the results of this study suggested that the detected pesticide residues in herbal decoctions could not be considered as posing a serious health risk. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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16 pages, 1843 KiB

Open AccessFeature PaperArticle

Development of a Novel LC-MS/MS Multi-Method for the Determination of Regulated and Emerging Food Contaminants Including Tenuazonic Acid, a Chromatographically Challenging Alternaria Toxin

by Ádám Tölgyesi, Attila Cseh, Andrea Simon and Virender K. Sharma

Molecules 2023, 28(3), 1468; https://doi.org/10.3390/molecules28031468 - 02 Feb 2023

Cited by 3 | Viewed by 2021

Abstract

The regulation of food contaminants in the European Union (EU) is comprehensive, and there are several compounds in the register or being added to the recommendation list. Recently, European standard methods for analysis have also been issued. The quick analysis of different groups [...] Read more.

The regulation of food contaminants in the European Union (EU) is comprehensive, and there are several compounds in the register or being added to the recommendation list. Recently, European standard methods for analysis have also been issued. The quick analysis of different groups of analytes in one sample requires a number of methods and the simultaneous use of various instruments. The aim of the present study was to develop a method that could analyze several groups of food contaminants: in this case, 266 pesticides, 12 mycotoxins, 14 alkaloid toxins, and 3 Alternaria toxins. The main advantage of the herein described approach over other methods is the simultaneous analysis of tenuazonic acid (TEA) and other relevant food contaminants. The developed method unites the newly published standard methods such as EN 15662:2018, EN 17194:2019, EN 17256:2019, EN 17425:2021, EN 17521:2021, which describes the analysis of both regulated and emerging contaminants. The developed method is based on a QuEChERS sample preparation, followed by LC-MS/MS analysis under alkaline mobile phase conditions. The pH of the aqueous eluent was set to 8.3, which resulted in baseline separation among ergot alkaloids and their corresponding epimers, a symmetric chromatographic peak shape for analyzing TEA and fit-for-purpose sensitivity for MS/MS detection in both positive and negative ionization modes. Those compounds, which possess the corresponding isotopically labeled internal standards (ISTD), allowed for direct quantification by the developed method and no further confirmation was necessary. This was proven by satisfactory analyses of a number of quality control (QC), proficiency test (PT), and validation samples. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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19 pages, 2769 KiB

Open AccessArticle

Risk Assessment of Pesticide Residues by GC-MSMS and UPLC-MSMS in Edible Vegetables

by Mohamed T. Selim, Mohammad M. Almutari, Hassan I. Shehab and Mohamed H. EL-Saeid

Molecules 2023, 28(3), 1343; https://doi.org/10.3390/molecules28031343 - 31 Jan 2023

Cited by 3 | Viewed by 2193

Abstract

In recent years, there has been a significant increase related to pesticide residues in foods, which may increase the risks to the consumer of these foods with the different quality and concentrations of pesticide residues. Pesticides are used for controlling pests that reduce [...] Read more.

In recent years, there has been a significant increase related to pesticide residues in foods, which may increase the risks to the consumer of these foods with the different quality and concentrations of pesticide residues. Pesticides are used for controlling pests that reduce yields. On the other hand, it has become a major public health concern due to its toxic properties. Thus, the objective of the current study employed the application of Quick Easy Cheap Effective Rugged Safe (QuEChERS) method, in combination with gas and liquid chromatography-tandem mass spectrometric detection (GCMSMS, LCMSMS) in order to determine 137 pesticide residues (63 insecticides, 41 acaricides, 40 herbicide, 55 fungicide, nematicide, growth regulator, Chitin synthesis inhibitors, and Juvenile hormone mimics), in 801 vegetables such as 139 tomatoes, 185 peppers, 217 squash, 94 eggplants, and 166 cucumbers from different locations in Hail and Riyadh cities. The results showed that the majority of pesticide residues were detected for each of the following pesticides: acetaimpride, metalaxyl, imidaclopride, bifenthrin, pyridaben, difenoconazole, and azoxystrobien, which were repeated in the samples studied 39, 21, 11, 10, 8, 7, and 5, respectively. In addition, results observed that the tomato was the most contaminated with pesticide residues; it was contaminated with 19 compounds and was followed by pepper, cucumber, and squash, and the last commodity in the contaminated ranking was eggplant. The highest calculated estimated daily intakes (EDIs) were recorded for tomatoes which were estimated between 0.013 to 0.516 mg/kg of body weight per day (bw/day) while the lowest EDIs value was between 0.000002 to 0.0005 mg/kg of bw/day for cucumber. Results indicated that the EDIs values were lower than the acceptable daily intake (ADI) values. Results observed that the most of pesticide residues exposure in food consumption in Saudi Arabia were lower than ADIs. In addition, the highest value for health risk index (HRI) was recorded with Ethion residue in tomato, but in sweet pepper, the highest value for HRI was 127.5 in the form of fipronil residue. On the other hand, results found that the highest values of HRI were 1.54, 1.61, and 0.047 for difenoconazole, bifenthrin, and pyridaben residues in squash, eggplant, and cucumber. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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14 pages, 2212 KiB

Open AccessArticle

Ionic Liquid-Dispersive Micro-Extraction and Detection by High Performance Liquid Chromatography–Mass Spectrometry for Antifouling Biocides in Water

by Li Zhou, Tong Wu, Chuanshan Yu, Shaowen Liu and Canping Pan

Molecules 2023, 28(3), 1263; https://doi.org/10.3390/molecules28031263 - 28 Jan 2023

Cited by 2 | Viewed by 1479

Abstract

A simple analytical method was developed and evaluated for the determination of two antifouling biocides using an ionic liquid-dispersive liquid–liquid micro-extraction (IL-DLLME) and a high-performance liquid chromatography–electrospray ionization mass spectrometry (LC-ESI-MS) analysis. Irgarol 1051 and Sea-Nine 211 were extracted from deionized water, lake [...] Read more.

A simple analytical method was developed and evaluated for the determination of two antifouling biocides using an ionic liquid-dispersive liquid–liquid micro-extraction (IL-DLLME) and a high-performance liquid chromatography–electrospray ionization mass spectrometry (LC-ESI-MS) analysis. Irgarol 1051 and Sea-Nine 211 were extracted from deionized water, lake water, and seawater using IL 1-hexyl-3-methylimidazolium hexafluorophosphate ([HMIm][PF6]) and ethyl acetate as the extraction solvent and the dispersion solvent. Several factors were considered, including the type and volume of extraction and dispersive solvent, IL amount, sample pH, salt effect, and cooling temperature. The developed method resulted in a recovery range of 78.7–90.3%, with a relative standard deviation (RSD, n = 3) less than 7.5%. The analytes were enriched greater than 40-fold, and the limits of detection (LOD) for two antifouling biocides were 0.01–0.1 μg L⁻¹. The method was effectively applied for the analysis of real samples of freshwater as well as samples of seawater. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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10 pages, 1891 KiB

Open AccessArticle

Monitoring and Exposure Assessment of Fosetyl Aluminium and Other Highly Polar Pesticide Residues in Sweet Cherry

by Emrah Gormez, Ozgur Golge, Miguel Ángel González-Curbelo and Bulent Kabak

Molecules 2023, 28(1), 252; https://doi.org/10.3390/molecules28010252 - 28 Dec 2022

Cited by 3 | Viewed by 1699

Abstract

Cherries are popular fruits due to their health benefits, organoleptic quality, and attractive appearance. Since highly polar pesticides are of low mass and amphoteric character, and are not amenable to traditional multi-residue extraction methods, they are more commonly not included in the pesticide [...] Read more.

Cherries are popular fruits due to their health benefits, organoleptic quality, and attractive appearance. Since highly polar pesticides are of low mass and amphoteric character, and are not amenable to traditional multi-residue extraction methods, they are more commonly not included in the pesticide monitoring program. This study aims to determine twelve highly polar pesticide residues in cherry samples intended for export from Turkey. A total of 16,022 cherry samples from 2018–2020 harvests in four production areas of Turkey were analyzed using a modification of the Quick Polar Pesticides method and liquid chromatography-tandem mass spectrometry. The method was validated at two fortification levels (0.01 and 0.05 mg kg⁻¹), and good recoveries (87.4–111.4%) and relative standard deviations (<6%) were achieved for all analytes. The limits of quantification were in the range of 1.08–2.55 μg kg⁻¹. Overall, 28.4% of the analyzed cherry samples were detected with phosphonic acid, calculated as fosetyl aluminium (fosetyl-Al) in amounts up to 77.7 mg kg⁻¹. For 2304 samples (14.4%), the residues exceeded the European Union maximum residue level of 2 mg kg⁻¹. There is no reason to be concerned about long-term exposure to phosphonic acid/fosetyl-Al, and the other highly polar pesticides through the consumption of sweet cherry. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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13 pages, 2197 KiB

Open AccessArticle

Stable Isotope Analysis of Residual Pesticides via High Performance Liquid Chromatography and Elemental Analyzer–Isotope Ratio Mass Spectrometry

by Hee Young Yun, Eun-Ji Won, Jisoo Choi, Yusang Cho, Da-Jung Lim, In-Seon Kim and Kyung-Hoon Shin

Molecules 2022, 27(23), 8587; https://doi.org/10.3390/molecules27238587 - 06 Dec 2022

Cited by 4 | Viewed by 1685

Abstract

To broaden the range of measurable pesticides for stable isotope analysis (SIA), we tested whether SIA of the anthranilic diamides cyantraniliprole (CYN) and chlorantraniliprole (CHL) can be achieved under elemental analyzer/isotope ratio mass spectrometry with compound purification in high-performance liquid chromatography (HPLC). Using [...] Read more.

To broaden the range of measurable pesticides for stable isotope analysis (SIA), we tested whether SIA of the anthranilic diamides cyantraniliprole (CYN) and chlorantraniliprole (CHL) can be achieved under elemental analyzer/isotope ratio mass spectrometry with compound purification in high-performance liquid chromatography (HPLC). Using this method, carbon isotope compositions were measured in pesticide residues extracted from plants (lettuce) grown indoors in potting soil that were treated with 500 mg/kg CHL and 250 mg/kg CYN and were followed up for 45 days. Our results show that the CYN and CHL standard materials did not have significant isotope differences before and after clean-up processing in HPLC. Further, when applied to the CYN product and CHL product in soil, stable isotope differences between the soil and plant were observed at <1.0‰ throughout the incubation period. There was a slight increase in the variability of pesticide isotope ratio detected with longer-term incubation (CHL, on average 1.5‰). Overall, we measured the carbon isotope ratio of target pesticides from HPLC fraction as the purification and pre-concentration step for environmental and biological samples. Such negligible isotopic differences in pesticide residues in soils and plants 45 days after application confirmed the potential of CSIA to quantify pesticide behavior in environments. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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20 pages, 1423 KiB

Open AccessArticle

Pesticide Residues in Vegetables and Fruits from Farmer Markets and Associated Dietary Risks

by El-Sayed A. El-Sheikh, Mahmoud M. Ramadan, Ahmed E. El-Sobki, Ali A. Shalaby, Mark R. McCoy, Ibrahim A. Hamed, Mohamed-Bassem Ashour and Bruce D. Hammock

Molecules 2022, 27(22), 8072; https://doi.org/10.3390/molecules27228072 - 21 Nov 2022

Cited by 21 | Viewed by 6475

Abstract

The use of pesticides leads to an increase in agricultural production but also causes harmful effects on human health when excessively used. For safe consumption, pesticide residues should be below the maximum residual limits (MRLs). In this study, the residual levels of pesticides [...] Read more.

The use of pesticides leads to an increase in agricultural production but also causes harmful effects on human health when excessively used. For safe consumption, pesticide residues should be below the maximum residual limits (MRLs). In this study, the residual levels of pesticides in vegetables and fruits collected from farmers’ markets in Sharkia Governorate, Egypt were investigated using LC-MS/MS and GC-MS/MS. A total number of 40 pesticides were detected in the tested vegetable and fruit samples. Insecticides were the highest group in detection frequency with 85% and 69% appearance in vegetables and fruits, respectively. Cucumber and apple samples were found to have the highest number of pesticide residues. The mean residue levels ranged from 7 to 951 µg kg⁻¹ (in vegetable samples) and from 8 to 775 µg kg⁻¹ (in fruit samples). It was found that 35 (40.7%) out of 86 pesticide residues detected in vegetables and 35 (38.9%) out of 90 pesticide residues detected in fruits exceeded MRLs. Results for lambda-cyhalothrin, fipronil, dimothoate, and omethoate in spinach, zucchini, kaki, and strawberry, respectively, can cause acute or chronic risks when consumed at 0.1 and 0.2 kg day⁻¹. Therefore, it is necessary for food safety and security to continuously monitor pesticide residues in fruits and vegetables in markets. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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10 pages, 2651 KiB

Open AccessArticle

Determination of Cyclaniliprole in Fruits and Vegetables Using Disposable Pipette Extraction Cleanup and Ultrahigh-Performance Liquid Chromatography-Tandem Mass Spectrometry

by Zhou Lu, Weiqian Yue, Weiming Ren, Yanhong Wang and Yueru Li

Molecules 2022, 27(19), 6464; https://doi.org/10.3390/molecules27196464 - 30 Sep 2022

Cited by 1 | Viewed by 1377

Abstract

Despite an outstanding agent for control of Lepidoptera, the diamide insecticide cyclaniliprole (CYCP) is a suspected carcinogen. In the present study, an analytical method was developed for the determination of CYCP in six fruits and vegetables (apple, grape, peach, bell pepper, lettuce, and [...] Read more.

Despite an outstanding agent for control of Lepidoptera, the diamide insecticide cyclaniliprole (CYCP) is a suspected carcinogen. In the present study, an analytical method was developed for the determination of CYCP in six fruits and vegetables (apple, grape, peach, bell pepper, lettuce, and tomato) using ultrahigh-performance liquid chromatography coupled with tandem mass spectrometry. Sample preparation was carried out by the acetonitrile-salting-out extraction followed by simple and fast cleanup of disposable pipette extraction tip containing styrene divinyl benzene and/or graphitized carbon black. Satisfactory linearity (r > 0.99) was obtained in the calibration range of 0.001–1 µg mL⁻¹. Matrix effects decreased from −9.9–−17.9% to −1.0–−7.6% after the cleanup. The recoveries of CYCP at three spike levels (0.01, 0.1, and 1 mg kg⁻¹) from different matrices were between 75.7% and 111.5%, with the intra-day (n = 5) and inter-day (n = 15) relative standard deviations lower than 12.1%. The limit of quantification was 0.01 mg kg⁻¹. The developed method provides a good reference for routine monitoring of CYCP in these fruits and vegetables. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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13 pages, 2228 KiB

Open AccessArticle

Simultaneous Preconcentration of Triazole Fungicide Residues Using In-Situ Coacervative Extraction Based on a Double-Solvent Supramolecular System Prior to High Performance Liquid Chromatographic Analysis

by Rachaya Buppasang, Jaruwan Palasak, Rawikan Kachangoon, Kraingkrai Ponhong, Norio Teshima, Rodjana Burakham, Supalax Srijaranai and Jitlada Vichapong

Molecules 2022, 27(19), 6273; https://doi.org/10.3390/molecules27196273 - 23 Sep 2022

Cited by 4 | Viewed by 1161

Abstract

An in situ coacervative extraction (IS-CAE) based on a double-solvent supramolecular system coupled to liquid–liquid microextraction is investigated for extraction and enrichment of triazole fungicides. The formation of a double-solvent supramolecular system was generated by in situ formation and used as an extraction [...] Read more.

An in situ coacervative extraction (IS-CAE) based on a double-solvent supramolecular system coupled to liquid–liquid microextraction is investigated for extraction and enrichment of triazole fungicides. The formation of a double-solvent supramolecular system was generated by in situ formation and used as an extraction solvent for the coacervative extraction method. No disperser solvent was required. This new double-solvent supramolecular system has a higher extraction ability than any of its components alone. The different factors that could affect the extraction capability were studied and optimized, including the type of double extractant and its volume, salt addition, vortex time, and centrifugation time. Under optimum extraction conditions, this method provides high enrichment factors (EFs) of 73–318 with low limits of detection (LODs) of 0.3–1 μg L⁻¹ and limits of quantitation (LOQs) of 1–3 μg L⁻¹. In addition, the proposed method was prosperously applied for the determination of triazole fungicides in water, fruit juice, and soy milk samples. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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12 pages, 801 KiB

Open AccessArticle

Dissipation, Processing Factors and Dietary Risk Assessment for Flupyradifurone Residues in Ginseng

by Nan Fang, Changpeng Zhang, Zhongbin Lu, Zhou Lu, Zhongbei Zhang, Bo Wang, Zhiguang Hou and Xueping Zhao

Molecules 2022, 27(17), 5473; https://doi.org/10.3390/molecules27175473 - 26 Aug 2022

Cited by 8 | Viewed by 1343

Abstract

The massive use of pesticides has brought great risks to food and environmental safety. It is necessary to develop reliable analytical methods and evaluate risks through monitoring studies. Here, a method was used for the simultaneous determination of flupyradifurone (FPF) and its two [...] Read more.

The massive use of pesticides has brought great risks to food and environmental safety. It is necessary to develop reliable analytical methods and evaluate risks through monitoring studies. Here, a method was used for the simultaneous determination of flupyradifurone (FPF) and its two metabolites in fresh ginseng, dried ginseng, ginseng plants, and soil. The method exhibited good accuracy (recoveries of 72.8–97.5%) and precision (relative standard deviations of 1.1–8.5%). The field experiments demonstrated that FPF had half-lives of 4.5–7.9 d and 10.0–16.9 d in ginseng plants and soil, respectively. The concentrations of total terminal residues in soil, ginseng plants, dried ginseng, and ginseng were less than 0.516, 2.623, 2.363, and 0.641 mg/kg, respectively. Based on these results, the soil environmental risk assessment shows that the environmental risk of FPF to soil organisms is acceptable. The processing factors for FPF residues in ginseng were 3.82–4.59, indicating that the concentration of residues increased in ginseng after drying. A dietary risk assessment showed that the risk of FPF residues from long-term and short-term dietary exposures to global consumers were 0.1–0.4% and 12.07–13.16%, respectively, indicating that the application of FPF to ginseng at the recommended dose does not pose a significant risk to consumers. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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Review

Jump to: Research, Other

23 pages, 3337 KiB

Open AccessReview

Pesticide-Residue Analysis in Soils by the QuEChERS Method: A Review

by Miguel Ángel González-Curbelo, Diana Angélica Varela-Martínez and Diego Alejandro Riaño-Herrera

Molecules 2022, 27(13), 4323; https://doi.org/10.3390/molecules27134323 - 05 Jul 2022

Cited by 26 | Viewed by 4538

Abstract

Pesticides are among the most important contaminants worldwide due to their wide use, persistence, and toxicity. Their presence in soils is not only important from an environmental point of view, but also for food safety issues, since such residues can migrate from soils [...] Read more.

Pesticides are among the most important contaminants worldwide due to their wide use, persistence, and toxicity. Their presence in soils is not only important from an environmental point of view, but also for food safety issues, since such residues can migrate from soils to food. However, soils are extremely complex matrices, which present a challenge to any analytical chemist, since the extraction of a wide range of compounds with diverse physicochemical properties, such as pesticides, at trace levels is not an easy task. In this context, the QuEChERS method (standing for quick, easy, cheap, effective, rugged, and safe) has become one of the most green and sustainable alternatives in this field due to its inherent advantages, such as fast sample preparation, the minimal use of hazardous reagents and solvents, simplicity, and low cost. This review is aimed at providing a critical revision of the most relevant modifications of the QuEChERS method (including the extraction and clean-up steps of the method) for pesticide-residue analysis in soils. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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28 pages, 5540 KiB

Open AccessConcept Paper

Quality Control of Pesticide Residue Measurements and Evaluation of Their Results

by Árpád Ambrus, Vy Vy Ngoc Doan, Júlia Szenczi-Cseh, Henriett Szemánné-Dobrik and Adrienn Vásárhelyi

Molecules 2023, 28(3), 954; https://doi.org/10.3390/molecules28030954 - 18 Jan 2023

Cited by 3 | Viewed by 2067

Abstract

Pesticide residues are monitored in many countries around the world. The main aims of the programs are to provide data for dietary exposure assessment of consumers to pesticide residues and for verifying the compliance of the residue concentrations in food with the national [...] Read more.

Pesticide residues are monitored in many countries around the world. The main aims of the programs are to provide data for dietary exposure assessment of consumers to pesticide residues and for verifying the compliance of the residue concentrations in food with the national or international maximum residue limits. Accurate residue data are required to reach valid conclusions in both cases. The validity of the analytical results can be achieved by the implementation of suitable quality control protocols during sampling and determination of pesticide residues. To enable the evaluation of the reliability of the results, it is not sufficient to test and report the recovery, linearity of calibration, the limit of detection/quantification, and MS detection conditions. The analysts should also pay attention to and possibly report the selection of the portion of sample material extracted and the residue components according to the purpose of the work, quality of calibration, accuracy of standard solutions, and reproducibility of the entire laboratory phase of the determination of pesticide residues. The sources of errors potentially affecting the measured residue values and the methods for controlling them are considered in this article. Full article

(This article belongs to the Special Issue Chromatographic Analysis of Pesticide in Environmental and Food)

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