BULLETIN OF ENVIRONMENTAL CONTAMINATION AND TOXICOLOGY
·
2023
·Vol. 111
·期 4
·1-9
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IF 2.7
Zheng Handinghong,Wu Qiong,Wu Xiaomao
This study aimed to investigate the dissipation, residues and dietary assessment of kresoxim-methyl in the application of Rosa Roxburghii and soil field using liquid chromatography-tandem mass spectrometry (LC–MS/MS). The results show that kresoxim-methyl in R. roxburghii samples was extracted by acetonitrile and purified by ethyl enediamine-N-propylsilane (PSA), while kresoxim-methyl in soil samples was extracted by acetonitrile and purified by octadecylsilyl solid phase dispersant (C 18 ). 0.1% formic acid (v/v)-water–methanol solution was used as the mobile phase, LC–MS/MS exhibited a good linearity in the range of 0.001–10 mg L −1 . The recoveries of R. roxburghii and soil matrix were 82.48%–102.55%, and the relative standard deviation ( RSD) were 1.13%–4.21%. The limit of detection ( LOD ) and quantification ( LOQ ) of kresoxim-methyl in R. roxburghii and soil samples was 0.50 and 0.60 µg kg −1 , respectively. The dissipation dynamics of kresoxim-methyl in R. roxburghii and soil followed the first-order kinetics, with the half-life of 4.28 and 4.41 days, respectively. The terminal residual amount of kresoxim-methyl in R. roxburghii and soil samples was 0.003–1.764 and 0.007–2.091 mg kg −1 , respectively. The dietary intake risk assessment indicates that a risk quotient ( RQ ) for kresoxim-methyl based on the national estimated daily intake ( NEDI ) of 0.1995 mg was 0.79%, suggesting that the use of kresoxim-methyl on R. roxburghii at recommended dosage was safe to consumers. This study provides the theoretical basis for guiding the rational use of kresoxim-methyl in the production of R. roxburghii .
研究领域:
植物学
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农业科学
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食品科学
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MICROCHEMICAL JOURNAL
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2026
·
IF 5.2
Xu Xu,Yumeng Liu,Jia Lv,Baocheng Ji,Junguang Li,Ke Li,Dianbo Zhao,Yanhong Bai
A modified QuEChERS method was developed in analysis of 52 veterinary drugs. • A novel MIL-101(Cr)–rGO@melamine sponge composite was fabricated. • The fast matrix purification could be achieved within several seconds. • Matrix cleanup was achieved through simple soaking and squeezing. • The method showed low matrix effects, good recoveries, and high precision. Herein, we report the fabrication of an elastic, quick, easy, cheap, effective, rugged, and safe adsorbent using a functionalized melamine sponge (MLS) and used it for the high-throughput analysis of 52 veterinary drugs in beef liver samples via ultraperformance liquid chromatography–tandem mass spectrometry. The as-prepared adsorbent was obtained by successive loading of Matérial Institut Lavoisier-101 (Chromium) [MIL-101(Cr)] and reduced graphene oxide (rGO) on melamine sponge skeletons. Excellent linearity with determination coefficients of ≥0.9942 was obtained across a range of 0.25–200 μg·kg −1 . Relatively low limits of detection (0.1–4.9 μg·kg −1 ) and limit of quantitation (LOQ; 0.3–16.2 μg·kg −1 ) were obtained. When fortified at three levels (1×, 5×, and 10× LOQ), spiked recoveries varied between 63.5% and 115.4%, with the intraday and interday relative standard deviations of ≤12.9%. Through direct infiltration and compression, efficient matrix purification was accomplished within seconds, yielding negligible matrix effects (from −18.4% to +19.1%). Thus, the MIL-101(Cr)–rGO@MLS adsorbent possesses high potential for fast, convenient, and efficient matrix purification in complex sample analysis. Download: Download high-res image (179KB) Download: Download full-size image
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JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Jing Lin,Dan Li,Peiyuan Luo,Laisheng Li
we reported a new phenylcarbamoylethylenediureido-β-cyclodextrin CSP (PUCDP) for HPLC, which was conveniently prepared by immobilizing the addition product of diethylenetriamino-β-CD with 3,5-dichlorophenyl isocyanate onto silica gel. After structural characterization, the chromatographic performance of PUCDP was preliminarily evaluated by using common 11 triazole pesticides as probes. The results showed that PUCDP had strong chiral separation abilities for all triazoles ( R s=1.44–3.70). Especially, it could first completely separate triazoles with two chiral centers such as cyproconazole, triadimenol, metconazole, paclobutrazol and bitertanol, into four peaks, respectively. Some effects on the separation and detection were investigated, including the composition of mobile phase, pH value, column temperature, and absorption wavelength. Based on comprehensive optimization of chromatographic conditions and a homemade PUCDP column, we established a new method for the simultaneous separation and determination of twelve triazole pesticide enantiomeric residues (flutriafol, cyproconazole, tebuconazole, and metconazole) in nine kinds of fruits and vegetables (apple, banana, orange, pear, cucumber, green pepper, tomato, wax gourd, cabbage). After simple QuEChERS pretreatment, samples were analyzed under the optimized conditions of a gradient elution program with acetonitrile-water (ACN H 2 O) containing 0.5 % triethylammonium acetate (TEAA) buffer (pH=6.30) as the mobile phase at a flow rate of 0.5 mL min -1 , a photo-diode array (PDA) detector at 220 nm, column temperature at 20 °C and an injection volume of 20 μL. The method exhibited good linear relationship ( R 2 =0.9941–0.9999) in the range of 0.5–60 mg l -1 for all triazole enantiomers. The limits of detection (LODs) and limits of quantification (LOQs) ranged from 0.05 to 0.10 mg kg -1 and 0.15 to 0.30 mg kg -1 , respectively. The average recoveries of all enantiomers were 81.60 %-104.08 % with intra -day and inter -day relative standard deviations (RSDs) of 1.91 %-3.50 % ( n = 5) and 2.05 %-4.49 % ( n = 15), respectively. The determination of 54 actual samples indicated the practicality of the method. This simultaneous determination method could save analysis time, and reduce solvent consumption with high analysis efficiency. The excellent performance of PUCDP was mainly related to the rich hydrogen bonds (donors and acceptors), the large π-π stacking and the extended cavity derived from the diphenylurea groups, which was consistent with the results of AutoDock molecular docking.
研究领域:
分析化学
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色谱技术
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农药残留分析
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食品安全
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手性分离技术
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高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2026
·
IF 5.3
Xiuli Ren,Yunheng Yao,Xinzi Wu,Lunpeng Wu,Hanghong Guo,Nanzhe Jiang
In this study, a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the simultaneous quantification of 16 pesticide residues in three typical vegetable matrices, using amino-functionalized halloysite nanotubes (HNTs-NQ-62) as a novel cleanup adsorbent. Three modified HNTs, namely HNTs-KH-540, HNTs-KH-792, and HNTs-NQ-62, were synthesized and systematically compared. The results demonstrated that HNTs-NQ-62 yielded lower matrix effects (MEs) values than HNTs-KH-540 and HNTs-KH-792 and exhibited a greater capacity to alleviate matrix interferences. Method validation confirmed that the proposed method achieved favorable linearity, with correlation coefficients ( R 2 ) higher than 0.9989 for all target pesticides. The limits of detection (LODs) and quantification (LOQs) ranged from 0.02 to 1.5 μg/kg and from 0.06 to 5.0 μg/kg, respectively. Satisfactory recoveries of 80.8%-113.7% were obtained, while the intraday and interday relative standard deviations (RSDs) were below 8.8% and 7.2%, respectively. Comparative tests further revealed that HNTs-NQ-62 performed better than the commercial adsorbent in mitigating MEs to a certain extent. This study indicates that HNTs-NQ-62 holds a great promise as a favorable alternative to conventional QuEChERS cleanup adsorbents and that the developed method provides reliable analytical performance for the quantification of the 16 target pesticides in vegetable matrices.
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Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment
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2020
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IF 2.34
Kai Cui,Xiaohu Wu,Lusheng Zhu,Ying Zhang,Gaochen Dai,Junli Cao,Jun Xu,Fengshou Dong,Xingang Liu,Yongquan Zheng
In this study, we established a rapid and sensitive HPLC-MS/MS method for quantitative determination of tembotrione and its metabolite AE 1417268 (M5) in corn, corn oil, beef, pork, chicken, and eggs. Both analytes eluted from a C18 column within 6 min. The electrospray ionisation–positive mode was used for tembotrione, whereas the negative mode was used for M5. Acetonitrile was the extractant for all samples, and the addition of 2 g NaCl to each homogenised sample facilitated the extraction of the analytes into acetonitrile. The extracted analytes were further purified by the addition of 50 mg of C18 sorbent (25 mg GCB was also added to corn samples) for subsequent HPLC-MS/MS analysis. Satisfactory calibration-curve linearities (R2 ≥ 0.997) were obtained for the two analytes at concentrations of 1–500 μg/L. Mean recoveries in different matrices ranged from 73.7% to 110.4%, whereas intra-day and inter-day relative standard deviations were <15% for all concentrations of spiked analytes. The limit of quantification was 2 μg/kg for each analyte in all matrices. In food samples obtained from markets, residual tembotrione and M5 were all below the limits of quantification. These results confirm that the method is suitable for the routine monitoring of residual tembotrione and M5 in a variety of food matrices.
研究领域:
食品科学
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分析化学
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JOURNAL OF CHROMATOGRAPHY A
·
2023
·
IF 4.1
Youzhi Su,Jianjiang Lu,Fang Li,Jun Liu
The establishment of an analytical method for pesticide residues in livestock urine can realize the real-time monitoring of pesticide pollution in livestock breeding. In this study, a novel method was developed for the determination of 106 pesticide residues in livestock urine based on a modified QuEChERS extraction and liquid chromatography–tandem mass spectrometry. Acetonitrile was used to extract target analytes through acidic and alkaline switching of the sample environment. The purification effect of captiva EMR-Lipid on samples was investigated. Three kinds of materials, C 18 , polar enhanced polymer (PEP), N-propylethylenediamine (PSA), were selected from 20 kinds of materials as adsorbents for QuEChERS. A mass analysis was carried out using simultaneous scanning in both positive and negative ion mode and multiple reaction monitoring mode. All analytes showed good linearity, with correlation coefficients ( R 2 ) greater than 0.9923; their limits of quantification were 0.02–1.95 ng/mL. The average recoveries at low, medium, and high spiked levels were in the range of 70.1 %–117.3 %, with intra-day precision ranging from 3.4 % to 16.9 % and inter-day precision ranging from 4.0 % to 19.3 %. The established analytical method was used to analyze the pesticide residue in swine urine and bovine urine collected from farms in Yining, Xinjiang, China. A total of 8 pesticides were detected, and the residue ranged from less than the limit of quantitation to 22.4 ng/mL. The top three pesticides with the highest detection frequency were clothianidin , thiamethoxam , and dinotefuran . The exposure assessment based on the monitored pesticide residue concentration levels showed that the detected pesticides could pose little risk to cattle and pigs.
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
·
2019
·
IF 3.571
Xuejin Mao,Aiping Yan,Yiqun Wan,Dongmei Luo,Hongshun Yang
A QuEChERS-type method without matrix interference was designed and developed to determine organophosphorus pesticide residues in edible vegetable oils, based on dispersive solid-phase extraction with cleanup using UiO-66 as sorbent. Microporous UiO-66 directly and selectively adsorbed organophosphorus pesticides and excluded interfering compounds. Clean analytes were obtained by elution and analyzed using gas chromatography–tandem mass spectrometry. The dispersive solid-phase extraction conditions (amount of adsorbent, extraction time, desorption solvent volume, and elution time) were optimized. The limits of detection of the pesticides in vegetable oils were 0.16–1.56 ng/g. Under optimized conditions, the average pesticide recoveries were 81.1–113.5%. The intraday and interday relative standard deviations for analyte recovery were <8.2 and <13.9%, respectively. Thus, the method is reliable and could detect organophosphorus pesticide residues in edible vegetable oils. Furthermore, UiO-66 can be easily recycled and reused at least 10 times, reducing the cost of analysis.
研究领域:
分析化学
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食品安全
·
环境科学
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JOURNAL OF CHROMATOGRAPHY A
·
2023
·
IF 4.1
Shengdong Pan,Xiaohai Li,Xinwu Xu,Dandan Zhang,Zemin Xu
As production processes have evolved, airborne concentrations of benzene, toluene and xylene in many workplaces are already well below the occupational exposure limits. However, studies have shown that low levels of exposure to benzene, toluene and xylene can still cause health effects in people exposed occupationally. However, there is no literature on health risk assessment of internal exposure. In view of this, an analytical method based on quaternary amine-functionalized core-shell-shell magnetic polymers (QA-CSS-MPs) was developed for the determination of seven metabolites in urine by MSPE-UPLC-DAD-HRMS. Furthermore, an improved QuEChERS method for the extraction of seven metabolites from human urine samples was introduced for the first time and satisfactory extraction rates were achieved. In addition, QA-CSS-MPs microspheres with core-shell-shell structure were designed and synthesized, and the morphology, composition and magnetic properties of the materials were fully characterized to verify the rationality of the synthetic route. Subsequently, QA-CSS-MPs microspheres were used as magnetic solid-phase extraction (MSPE) adsorbents for the purification of urine extracts, and UPLC-DAD-HRMS was used for the detection of seven metabolites. As a result, this method allows the accurate determination of seven metabolites in urine samples over an ultra-wide concentration range (0.001–100 mg/L). Under optimal experimental conditions, i.e., 2% hydrochloric acid in urine for the hydrolysis and 20 mg of QA-CSS-MPs for 5 min purification, the spiked recoveries of the seven target metabolites ranged from 81.5% to 117.7% with RSDs of 1.0%–9.4%. The limits of detection (LODs, S/N≥3) for the established method were in the range of 0.2–0.3 μg/L. The developed method was applied to 254 human urine samples for the determination of seven metabolites. The results showed that the concentration distributions of three xylene metabolites in urine, 2-MHA, 3-MHA, 4-MHA and total MHA, showed statistically significant differences for occupational exposure ( p <0.001). In addition, the results of the internal exposure assessment showed that there is a high potential health risk associated with occupational exposure processes.
研究领域:
分析化学
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职业健康
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环境科学
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材料科学
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高影响因子
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