Research

13 pages, 1291 KiB

Open AccessArticle

Pesticide Residues and Health Risk Assessment in Tomatoes and Lettuces from Farms of Metropolitan Region Chile

by Sebastian Elgueta, Marcela Valenzuela, Marcela Fuentes, Pablo Meza, Juan Pablo Manzur, Shaofeng Liu, Guoqing Zhao and Arturo Correa

Molecules 2020, 25(2), 355; https://doi.org/10.3390/molecules25020355 - 15 Jan 2020

Cited by 33 | Viewed by 5202

Abstract

Over the last years, the detection of pesticide residues in the official food surveillance programs of Chile has been increased, mainly in fresh vegetables such as tomatoes and lettuces. The Metropolitana Region of Chile presents the highest detections in the country. The lack [...] Read more.

Over the last years, the detection of pesticide residues in the official food surveillance programs of Chile has been increased, mainly in fresh vegetables such as tomatoes and lettuces. The Metropolitana Region of Chile presents the highest detections in the country. The lack of evaluations of toxicological risks in human health have increased uncertainty of the potential effects of pesticides exposures in the Chilean population. This research aims to determinate health risks assessment of pesticide residues associated to tomatoes and lettuces produced in Metropolitana Region. The findings of this study reveal that tomatoes and lettuces cultivated in the MR show more than 50% of samples with one or multiple pesticides residues. From the total samples, 16% were over the Chilean Maximum Residue Levels (MRLs). The main pesticides detected in tomatoes and lettuces were methamidophos, methomyl, difenoconazole, cyprodinil and boscalid. The results obtained using the official data of the Ministry of Health of Chile (MINSAL) compared to the World Health Organization (WHO), describe relevant risks through the Estimated Daily Intakes (EDI), Hazard Quotients (HQ) and Hazard Index (HI) for the Chilean population due to high concentrations of methamidophos, methomyl and cyprodinil. More restrictions for the use of methamidophos, methomyl, difenoconazole, cyprodinil and boscalid and effective control programs should be implemented in order to mitigate the impacts on the Chilean population. Full article

(This article belongs to the Special Issue Analysis of Residues in Food and Environment)

► Show Figures

Graphical abstract

16 pages, 2548 KiB

Open AccessArticle

Development and Validation of an HPLC-ESI/MS/MS Method for the Determination of Amoxicillin, Its Major Metabolites, and Ampicillin Residues in Chicken Tissues

by Lan Chen, Bo Wang, Zhixiang Diao, Min Zhao, Kaizhou Xie, Peiyang Zhang, Xutang Wang, Tao Zhang and Jinyu Wang

Molecules 2019, 24(14), 2652; https://doi.org/10.3390/molecules24142652 - 22 Jul 2019

Cited by 9 | Viewed by 5436

Abstract

A method for the simultaneous analysis of amoxicillin (AMO), amoxicillin metabolites, and ampicillin residues in edible chicken muscle, liver, and kidney samples via high-performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI/MS/MS) was developed and verified. The extraction and purification procedures involved the extraction [...] Read more.

A method for the simultaneous analysis of amoxicillin (AMO), amoxicillin metabolites, and ampicillin residues in edible chicken muscle, liver, and kidney samples via high-performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI/MS/MS) was developed and verified. The extraction and purification procedures involved the extraction of the sample using a liquid-liquid extraction method with acetonitrile to eliminate the proteins. The chicken tissue extract was then injected directly onto an HPLC column coupled to a mass spectrometer with an ESI(+) source. The HPLC-ESI/MS/MS method was validated according to specificity, sensitivity, linearity, matrix effects, precision, accuracy, decision limit, detection capability, and stability, as defined by the European Union and Food and Drug Administration. The linearity was desirable, and the determination coefficients (r² values) ranged from 0.9968 and 0.9999. The limits of detection and limits of quantification were 0.10–2.20 μg/kg and 0.30–8.50 μg/kg, respectively. The decision limits were 57.71–61.25 μg/kg, and the detection capabilities were 65.41–72.50 μg/kg, and the recoveries of the four target analytes exceeded 75% at the limits of quantification and exceeded 83% at 25, 50, and 100 μg/kg (n = 6 at each level), confirming the reliability of this method for determining these analytes and providing a new detection technology. For real sample analysis, this experiment tested 30 chicken tissue samples, only one chicken muscle, liver, and kidney sample were contaminated with 5.20, 17.45, and 7.33 μg/kg of AMO values, respectively, while other target compounds were not detected in the 30 tested chicken tissue samples. Full article

(This article belongs to the Special Issue Analysis of Residues in Food and Environment)

► Show Figures

Graphical abstract

13 pages, 1848 KiB

Open AccessArticle

Dissipation Kinetics and the Pre-Harvest Residue Limits of Acetamiprid and Chlorantraniliprole in Kimchi Cabbage Using Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

by Jonghwa Lee, Byung Joon Kim, Eunhye Kim and Jeong-Han Kim

Molecules 2019, 24(14), 2616; https://doi.org/10.3390/molecules24142616 - 18 Jul 2019

Cited by 22 | Viewed by 3828

Abstract

The dissipation behaviors of acetamiprid and chlorantraniliprole in kimchi cabbages were studied under open-field conditions. A simple and rapid analytical method was developed using ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). The multiple reaction monitoring (MRM) conditions of two pesticides [...] Read more.

The dissipation behaviors of acetamiprid and chlorantraniliprole in kimchi cabbages were studied under open-field conditions. A simple and rapid analytical method was developed using ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). The multiple reaction monitoring (MRM) conditions of two pesticides were optimized to quantify and identify the pesticide residues. Sample preparation was performed by the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method. Average recovery rates at the different spiked levels (0.05 and 0.25 mg/kg) were in the range of 103.6–113.9% (acetamiprid) and 80.8–91.2% (chlorantraniliprole), and the relative standard deviations were ≤4.3% for all. The dissipation kinetics were assessed using first-order equations after spraying acetamiprid and chlorantraniliprole individually on kimchi cabbages. The biological half-lives in field 1 and 2 were 5.2 and 6.3 days (acetamiprid) and 10.0 and 15.2 days (chlorantraniliprole), respectively. Based on the dissipation equations, the pre-harvest residue limits (PHRLs) corresponding to each day before harvest were suggested as the guidelines to meet the MRL on harvest day. It was also predicted that the terminal residues observed after multiple sprayings (three and seven days) would be below the MRL when harvested, in compliance with the established pre-harvest intervals. Full article

(This article belongs to the Special Issue Analysis of Residues in Food and Environment)

► Show Figures

Figure 1

14 pages, 2800 KiB

Open AccessArticle

Pesticide Residues Identification by Optical Spectrum in the Time-Sequence of Enzyme Inhibitors Performed on Microfluidic Paper-Based Analytical Devices (µPADs)

by Ning Yang, Naila Shaheen, Liangliang Xie, Junjie Yu, Hussain Ahmad and Hanping Mao

Molecules 2019, 24(13), 2428; https://doi.org/10.3390/molecules24132428 - 02 Jul 2019

Cited by 14 | Viewed by 2943

Abstract

Pesticides vary in the level of poisonousness, while a conventional rapid test card only provides a general “absence or not” solution, which cannot identify the various genera of pesticides. In order to solve this problem, we proposed a seven-layer paper-based microfluidic chip, integrating [...] Read more.

Pesticides vary in the level of poisonousness, while a conventional rapid test card only provides a general “absence or not” solution, which cannot identify the various genera of pesticides. In order to solve this problem, we proposed a seven-layer paper-based microfluidic chip, integrating the enzyme acetylcholinesterase (AChE) and chromogenic reaction. It enables on-chip pesticide identification via a reflected light intensity spectrum in time-sequence according to the different reaction efficiencies of pesticide molecules and assures the optimum temperature for enzyme activity. After pretreatment of figures of reflected light intensity during the 15 min period, the figures mainly focused on the reflected light variations aroused by the enzyme inhibition assay, and thus, the linear discriminant analysis showed satisfying discrimination of imidacloprid (Y = −1.6525X − 139.7500), phorate (Y = −3.9689X − 483.0526), and avermectin (Y = −2.3617X − 28.3082). The correlation coefficients for these linearity curves were 0.9635, 0.8093, and 0.9094, respectively, with a 95% limit of agreement. Then, the avermectin class chemicals and real-world samples (i.e., lettuce and rice) were tested, which all showed feasible graphic results to distinguish all the chemicals. Therefore, it is feasible to distinguish the three tested kinds of pesticides by the changes in the reflected light spectrum in each min (15 min) via the proposed chip with a high level of automation and integration. Full article

(This article belongs to the Special Issue Analysis of Residues in Food and Environment)

► Show Figures

Figure 1

7 pages, 772 KiB

Open AccessArticle

Metal Concentration in Muscle and Digestive Gland of Common Octopus (Octopus vulgaris) from Two Coastal Site in Southern Tyrrhenian Sea (Italy)

by Andrea Ariano, Raffaele Marrone, Rebecca Andreini, Giorgio Smaldone, Salvatore Velotto, Serena Montagnaro, Aniello Anastasio and Lorella Severino

Molecules 2019, 24(13), 2401; https://doi.org/10.3390/molecules24132401 - 29 Jun 2019

Cited by 19 | Viewed by 2678

Abstract

Octopus vulgaris constitute an important part of most suitable marine resources for human consumption, however, they can represent a source in chemical contaminants intake such as heavy metals. In this scenario, the aim of the study was the evaluation of the concentration of [...] Read more.

Octopus vulgaris constitute an important part of most suitable marine resources for human consumption, however, they can represent a source in chemical contaminants intake such as heavy metals. In this scenario, the aim of the study was the evaluation of the concentration of lead (Pb), cadmium (Cd) and mercury (Hg) in the muscle and digestive gland of octopus caught from two different locations along Campania coast (Castellammare di Stabia and Napoli) and the estimation of their weekly human intake derived from the ingestion of octopus. Analysing 38 samples showed a higher concentration of Pb in the muscle of octopus in Castellammare di Stabia than in Napoli. No statistical differences were reported for Cd, Pb and Hg concentrations in the digestive gland of octopus between two sampling sites. Differences were observed between the two tissue types, with a higher level of Cd and Pb observed in the digestive gland compared with the muscle. Noteworthy, the consumption of muscle from Castellammare di Stabia could increase Pb intake in heavy consumers of local octopus. In conclusion, the present work determines that it is important to improve strategies to minimize environmental pollution sources in these areas. Full article

(This article belongs to the Special Issue Analysis of Residues in Food and Environment)

► Show Figures

Graphical abstract

22 pages, 1745 KiB

Open AccessArticle

Development and Optimisation of a Multiresidue Method for the Determination of 40 Anthelmintic Compounds in Environmental Water Samples by Solid Phase Extraction (SPE) with LC-MS/MS Detection

by Damien Mooney, Catherine Coxon, Karl G Richards, Laurence Gill, Per-Erik Mellander and Martin Danaher

Molecules 2019, 24(10), 1978; https://doi.org/10.3390/molecules24101978 - 22 May 2019

Cited by 17 | Viewed by 3939

Abstract

A comprehensive multiresidue method was developed and validated for the determination of 40 anthelmintic compounds, including 13 transformation products, in surface and groundwater samples at sub nanogram per litre (ng L⁻¹) levels. Anthelmintic residues were extracted from unfiltered water samples using [...] Read more.

A comprehensive multiresidue method was developed and validated for the determination of 40 anthelmintic compounds, including 13 transformation products, in surface and groundwater samples at sub nanogram per litre (ng L⁻¹) levels. Anthelmintic residues were extracted from unfiltered water samples using polymeric divinylbenzene solid phase extraction (SPE) cartridges, and eluted with methanol: acetone (50:50, v/v). Purified extracts were concentrated, filtered and injected for UHPLC-MS/MS determination. The method recovery (at a concentration representative of realistic expected environmental water levels based on literature review) ranged from 83–113%. The method was validated, at three concentration levels, in accordance to Commission Decision 2002/657/EC and SANTE/11813/2017 guidelines. Trueness and precision, under within-laboratory reproducibility conditions, ranged from 88–114% and 1.1–19.4%, respectively. The applicability of the method was assessed in a pilot study whereby 72 different surface and groundwater samples were collected and analysed for the determination of these 40 compounds for the first time in Ireland. This is the most comprehensive method available for the investigation of the occurrence of both anthelmintic parent compounds and their transformation products in raw, unfiltered environmental waters. Full article

(This article belongs to the Special Issue Analysis of Residues in Food and Environment)

► Show Figures

Graphical abstract

14 pages, 3464 KiB

Open AccessArticle

A Modified QuEChERS Method for Determination of Pyrethroid Residues in Traditional Chinese Medicine Oral Liquids by High-Performance Liquid Chromatography

by Yuge Hou, Hong Chen, Xin Li, Yiyi Liao, Makoto Tsunoda, Yingxia Zhang, Shiming Deng and Yanting Song

Molecules 2019, 24(8), 1470; https://doi.org/10.3390/molecules24081470 - 13 Apr 2019

Cited by 14 | Viewed by 3786

Abstract

Pyrethroid residues in traditional Chinese medicines have been a serious threat to the health and treatment of patients. However, because of the matrix complexity of traditional Chinese medicine, the detection of pyrethroid residues remains a challenge. Therefore, we developed a QuEChERS method coupled [...] Read more.

Pyrethroid residues in traditional Chinese medicines have been a serious threat to the health and treatment of patients. However, because of the matrix complexity of traditional Chinese medicine, the detection of pyrethroid residues remains a challenge. Therefore, we developed a QuEChERS method coupled with high-performance liquid chromatography and ultraviolet detection (HPLC-UV) for the determination of pyrethroid pesticides in three kinds of traditional Chinese medicine oral liquid preparations, and we investigated and optimized the extraction conditions. The matrix effect was estimated in the organic solvent and the actual samples by comparing the slopes of calibration curves, and the results showed that the matrix effect is not significant when using the modified QuEChERS method. The pyrethroid pesticides could be completely separated in 30 min. The linear correlation coefficients were more than 0.999, and the recoveries of all the pyrethroid pesticides ranged from 87.2% to 104.8%. The intra-day precisions (n = 5) were 2.44–4.62%, and the inter-day precisions (n = 5) were 1.06–3.02%. Moreover, the limits of detection were in the range of 0.007–0.018 ng mL⁻¹, while the limits of quantitation were in the range of 0.022–0.057 ng mL⁻¹. This simple, low-cost, and highly sensitive analytical method can be a potential tool for the analysis of pyrethroid residues in traditional Chinese medicine oral liquid preparations. Full article

(This article belongs to the Special Issue Analysis of Residues in Food and Environment)

► Show Figures

Figure 1

10 pages, 3628 KiB

Open AccessArticle

Quantitative Determination of Acetamiprid in Pollen Based on a Sensitive Enzyme-Linked Immunosorbent Assay

by Qingkui Fang, Quan Zu, Xiude Hua, Pei Lv, Wanwen Lin, Dahe Zhou, Zihan Xu, Jiarui Fan, Xiaohan Li and Haiqun Cao

Molecules 2019, 24(7), 1265; https://doi.org/10.3390/molecules24071265 - 01 Apr 2019

Cited by 17 | Viewed by 3313

Abstract

A sensitive biotinylated indirect competitive enzyme-linked immunosorbent assay (Bic-ELISA) was developed to detect acetamiprid pesticides in pollen, based on the heterogeneous coating antigen and biotinylated anti-acetamiprid monoclonal antibody. Under optimized experimental conditions, the detection limit for the Bic-ELISA was 0.17 ng/mL and the [...] Read more.

A sensitive biotinylated indirect competitive enzyme-linked immunosorbent assay (Bic-ELISA) was developed to detect acetamiprid pesticides in pollen, based on the heterogeneous coating antigen and biotinylated anti-acetamiprid monoclonal antibody. Under optimized experimental conditions, the detection limit for the Bic-ELISA was 0.17 ng/mL and the linear range was 0.25–25 ng/mL. The cross-reactivities could be regarded as negligible for the biotinylated antibodies with their analogues except for thiacloprid (1.66%). Analyte recoveries for extracts of spiked pollen (camellia pollen, lotus pollen, rape pollen) ranged from 81.1% to 108.0%, with intra-day relative standard deviations (RSDs) of 4.8% to 10.9%, and the average reproducibility was 85.4% to 110.9% with inter-assay and inter-assay RSDs of 6.1% to 11.7%. The results of Bic-ELISA methods for the Taobao’s website samples were largely consistent with HPLC-MS/MS. Therefore, the established Bic-ELISA methods would be conducive to the monitoring of acetamiprid in pollen. Full article

(This article belongs to the Special Issue Analysis of Residues in Food and Environment)

► Show Figures

Figure 1

15 pages, 2529 KiB

Open AccessArticle

A Novel Modified Electrode for Detection of the Food Colorant Sunset Yellow Based on Nanohybrid of MnO₂ Nanorods-Decorated Electrochemically Reduced Graphene Oxide

by Ziyu Ding, Peihong Deng, Yiyong Wu, Yaling Tian, Guangli Li, Jun Liu and Quanguo He

Molecules 2019, 24(6), 1178; https://doi.org/10.3390/molecules24061178 - 25 Mar 2019

Cited by 58 | Viewed by 3823

Abstract

The nanohybrid of electrochemically-reduced graphene oxide (ERGO) nanosheets decorated with MnO₂ nanorods (MnO₂ NRs) was modified on the surface of a glassy carbon electrode (GCE). Controlled potential reduction was applied for the reduction of graphene oxide (GO). The characterization was performed [...] Read more.

The nanohybrid of electrochemically-reduced graphene oxide (ERGO) nanosheets decorated with MnO₂ nanorods (MnO₂ NRs) was modified on the surface of a glassy carbon electrode (GCE). Controlled potential reduction was applied for the reduction of graphene oxide (GO). The characterization was performed by scanning electron microscopy, X-ray diffraction and cyclic voltammetry. Compared with the poor electrochemical response at bare GCE, a well-defined oxidation peak of sunset yellow (SY) was observed at the MnO₂ NRs-ERGO/GCE, which was attributed to the high accumulation efficiency as well as considerable electrocatalytic activity of ERGO and MnO₂ NRs on the electrode surface. The experimental parameters for SY detection were optimized in detail. Under the optimized experiment conditions, the MnO₂ NRs-ERGO/GCE showed good linear response to SY in concentration range of 0.01–2.0 μM, 2.0–10.0 μM and 10.0–100.0 μM with a detection limit of 2.0 nM. This developed method was applied for SY detection in soft drinks with satisfied detected results. Full article

(This article belongs to the Special Issue Analysis of Residues in Food and Environment)

► Show Figures

Figure 1

12 pages, 2161 KiB

Open AccessArticle

Single-Piece Solid Contact Cu²⁺-Selective Electrodes Based on a Synthesized Macrocyclic Calix[4]arene Derivative as a Neutral Carrier Ionophore

by Abd El-Galil E. Amr, Mohamed A. Al-Omar, Ayman H. Kamel and Elsayed A. Elsayed

Molecules 2019, 24(5), 920; https://doi.org/10.3390/molecules24050920 - 06 Mar 2019

Cited by 10 | Viewed by 3219

Abstract

Herein, a facile route leading to good single-walled carbon nanotubes (SWCNT) dispersion or poly (3,4-ethylenedioxythiophene)/poly(styrenesulfonate) (PEDOT/PSS) based single-piece nanocomposite membrane is proposed for trace determination of Cu²⁺ ions. The single-piece solid contact Cu²⁺-selective electrodes were prepared after drop casting the [...] Read more.

Herein, a facile route leading to good single-walled carbon nanotubes (SWCNT) dispersion or poly (3,4-ethylenedioxythiophene)/poly(styrenesulfonate) (PEDOT/PSS) based single-piece nanocomposite membrane is proposed for trace determination of Cu²⁺ ions. The single-piece solid contact Cu²⁺-selective electrodes were prepared after drop casting the membrane mixture on the glassy-carbon substrates. The prepared potentiometric sensors revealed a Nernstian response slope of 27.8 ± 0.3 and 28.1 ± 0.4 mV/decade over the linearity range 1.0 × 10⁻³ to 2.0 × 10⁻⁹ and 1.0 × 10⁻³ to 1.0 × 10⁻⁹ M with detection limits of 5.4 × 10⁻¹⁰ and 5.0 × 10⁻¹⁰ M for sensors based on SWCNTs and PEDOT/PSS, respectively. Excellent long-term potential stability and high hydrophobicity of the nanocomposite membrane are recorded for the prepared sensors due to the inherent high capacitance of SWCNT used as a solid contact material. The sensors exhibited high selectivity for Cu²⁺ ions at pH 4.5 over other common ions. The sensors were applied for Cu²⁺ assessment in tap water and different tea samples. The proposed sensors were robust, reliable and considered as appealing sensors for copper (II) detection in different complex matrices. Full article

(This article belongs to the Special Issue Analysis of Residues in Food and Environment)

► Show Figures

Graphical abstract

13 pages, 3634 KiB

Open AccessArticle

All Solid-State Poly (Vinyl Chloride) Membrane Potentiometric Sensor Integrated with Nano-Beads Imprinted Polymers for Sensitive and Rapid Detection of Bispyribac Herbicide as Organic Pollutant

by Nashwa S. Abdalla, Maha A. Youssef, H. Algarni, Nasser S. Awwad and Ayman H. Kamel

Molecules 2019, 24(4), 712; https://doi.org/10.3390/molecules24040712 - 16 Feb 2019

Cited by 27 | Viewed by 3560

Abstract

All-solid-state potentiometric sensors were prepared by using polyaniline (PANI) as the solid contact material. A film of PANI (thickness approximately being 0.25 µm) was deposited on a solid substrate (carbon screen printed platform). The PANI layer was subsequently coated with an ion-selective membrane [...] Read more.

All-solid-state potentiometric sensors were prepared by using polyaniline (PANI) as the solid contact material. A film of PANI (thickness approximately being 0.25 µm) was deposited on a solid substrate (carbon screen printed platform). The PANI layer was subsequently coated with an ion-selective membrane (ISM) containing uniform-sized molecularly imprinted nanoparticles to produce a solid-contact ion-selective electrode (SC/ISE) for bispyribac herbicide (sensor I). In addition, aliquat 336 was also used as an ion exchanger in plasticized PVC membrane (sensor II). The proposed sensors revealed a remarkably improved sensitivity towards bispyribac ions with anionic slopes of −47.8 ± 1.1 (r² = 0.9995) and −44.4 ± 1.4 (r² = 0.9997) mV/decade over a linear range 1.0 × 10⁻²–8.6 × 10⁻⁶ M, 1.0 × 10⁻²–9.0 × 10⁻⁶ M and detection limits of 1.33 and 1.81 µg/mL for sensors I and II, respectively.Selectivity of both sensors is significantly high for different common pesticides and inorganic anions. The potential stability of the SC/ISEs was studied using chronopotentiometry. Electrochemical impedance spectrometry was used to understand the charge-transfer mechanisms of the different types of ion-selective electrodes studied. The impedance response of the electrodes was modelled by using equivalent electrical circuits. The sensors were used for a direct measurement of the bispyribac content in commercial herbicide formulations and soil samples collected from agricultural lands planted with rice and sprayed with bispyribac herbicide. The results agree fairly well with data obtained using HPLC method. Full article

(This article belongs to the Special Issue Analysis of Residues in Food and Environment)

► Show Figures

Graphical abstract

16 pages, 794 KiB

Open AccessArticle

Determination of Selected Priority Pesticides in High Water Fruits and Vegetables by Modified QuEChERS and GC-ECD with GC-MS/MS Confirmation

by Maciej Tankiewicz

Molecules 2019, 24(3), 417; https://doi.org/10.3390/molecules24030417 - 24 Jan 2019

Cited by 34 | Viewed by 6520

Abstract

A modified quick, easy, cheap, efficient, rugged and safe (QuEChERS) method coupled to gas chromatography with electron capture detector (GC-ECD) was developed for simultaneous determination of selected electronegative pesticides in fruits and vegetables with high water content. The chosen compounds are commonly detected [...] Read more.

A modified quick, easy, cheap, efficient, rugged and safe (QuEChERS) method coupled to gas chromatography with electron capture detector (GC-ECD) was developed for simultaneous determination of selected electronegative pesticides in fruits and vegetables with high water content. The chosen compounds are commonly detected in fruit and vegetable crops, and some of their metabolites have even been found in human urine. In addition, some of them are known or suspected carcinogens according to the International Agency for Research of Cancer. Extraction and clean up parameters were optimized, thus the original QuEChERS method was modified to decrease solvent usage, in accordance with ‘green chemistry’ principles. The proposed methodology was validated in terms of selectivity, specificity, linearity, precision and accuracy. The obtained limits of detection (LODs) for all investigated pesticides ranged from 5.6 µg·kg⁻¹ to 15 µg·kg⁻¹ and limits of quantification (LOQs) from 17 µg·kg⁻¹ to 45 µg·kg⁻¹. The obtained data demonstrated the good reproducibility and stability of the procedure in the tested concentration range up to 10 mg·kg⁻¹, with relative standard deviations (RSDs) lower than 10%. Recoveries for spiked pear samples at LOQ level for each pesticide were from 90% to 107% with RSDs lower than 9.6%. The suitability of the developed procedure was tested on various fruit and vegetable samples available on the market at different seasons. The proposed methodology is applicable for detection and monitoring of selected pesticides not only in fruits and vegetables with high water content, but also in samples containing large amounts of pigments and dyes. Full article

(This article belongs to the Special Issue Analysis of Residues in Food and Environment)

► Show Figures

Graphical abstract

12 pages, 1324 KiB

Open AccessArticle

New Photodegradation Products of the Fungicide Fluopyram: Structural Elucidation and Mechanism Identification

by Tessema F. Mekonnen, Ulrich Panne and Matthias Koch

Molecules 2018, 23(11), 2940; https://doi.org/10.3390/molecules23112940 - 10 Nov 2018

Cited by 7 | Viewed by 4576

Abstract

Identifying the fate of agrochemicals is important to understand their potential risk for living organisms. We report here new photodegradation products (PPs) of the fungicide fluopyram. The PPs were produced by irradiating a fluopyram standard in 0.1% acetonitrile aqueous media by a 150-W [...] Read more.

Identifying the fate of agrochemicals is important to understand their potential risk for living organisms. We report here new photodegradation products (PPs) of the fungicide fluopyram. The PPs were produced by irradiating a fluopyram standard in 0.1% acetonitrile aqueous media by a 150-W medium pressure Hg-lamp that emits wavelengths between 200–280 nm. The structural elucidation of PPs was achieved by combining the retention time, isotopic pattern, targeted fragmentation, and accurate mass measurements using liquid chromatography-tandem mass spectrometry (LC-MS/MS) and high resolution-MS (HRMS). In addition to previously known PPs, seven new PPs of fluopyram were identified in this work: mainly dihydroxyl and hydroxylimide fluopyram as well as mono, di, and trihydroxyl lactam. Additionally, two PPs were found to be formed by rearrangement after the loss of H₂C=CH₂. Hence, the results of the work contribute to extending the current knowledge regarding the photoinduced fate of agrochemicals, and fluopyram in particular. Full article

(This article belongs to the Special Issue Analysis of Residues in Food and Environment)

► Show Figures

Figure 1

Journal Menu

Journal Browser

Analysis of Residues in Food and Environment

Share This Special Issue

Special Issue Editor

Special Issue Information

Keywords

Related Special Issue

Published Papers (13 papers)

Research

Further Information

Guidelines

MDPI Initiatives

Follow MDPI