Journal of Analytical Methods in Chemistry
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2017
·
IF 1.801
Chang Xu,Yiyi Liao,Chunyan Fang,Makoto Tsunoda,Yingxia Zhang,Yanting Song,Shiming Deng
In this paper, a novel method of QuEChERS-based extraction coupled with high-performance liquid chromatography has been developed for the simultaneous determination of ursolic acid (UA) and oleanolic acid (OA) in guava leaves. The QuEChERS-based extraction parameters, including the amount of added salt, vortex-assisted extraction time, and absorbent amount, and the chromatographic conditions were investigated for the analysis of UA and OA in guava leaves. Under the optimized conditions, the method showed good linearity over a range of 1–320 μg mL−1, with correlation coefficients above 0.999. The limits of detection of UA and OA were 0.18 and 0.36 μg mL−1, respectively. The intraday and interday precision were below 1.95 and 2.55%, respectively. The accuracies of the UA and OA determinations ranged from 97.4 to 111.4%. The contents of UA and OA in the guava leaf samples were 2.50 and 0.73 mg g−1, respectively. These results demonstrate that the developed method is applicable to the simultaneous determination of UA and OA in guava leaves.
研究领域:
分析化学
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植物化学
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药物分析
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PubMed
高影响因子
TALANTA
·
2016
·
IF 4.035
Xiao-Chen Wang,Bin Shu,Shan Li,Zhao-Guang Yang,Bo Qiu
A fast, sensitive and environmental-friendly method was developed to determine 13 organochlorine pesticides in fish tissue through gas chromatography with electron capture detection. Sample was extracted initially by acetonitrile and then concentrated through dispersive liquid–liquid microextraction based on solidification of floating organic droplet (DLLME–SFO). Dispersive solid phase extraction (d-SPE) was not a separate step but integrated to DLLME-SFO procedure. In order to separate the d-SPE sorbent , water and organic phase well, a modification to the glass centrifuge tube was made to achieving high centrifugal speed. The optimized method was validated with recoveries ranging from 88.1% to 121.2% (with relative standard deviations <15%) at three spiked levels for all of the pesticides. Good linearity was achieved at seven concentration levels from 6.25 to 625 μg L −1 , which corresponded to 0.001–0.100 mg kg −1 in the sample. The limits of quantification and the limits of detection for 13 OCPs ranged from 1.94×10 −3 to 4.93×10 −3 mg kg −1 and 6.50×10 −4 to 1.58×10 −3 mg kg −1 , respectively. The method was successfully applied to analyze real fish samples.
研究领域:
分析化学
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环境科学
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食品安全
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PubMed
高影响因子
ACS Omega
·
2023
·
IF 4.1
Yue Chen,Deliang Gao,Yueming Wu,Ling Wang,Weidi Fan,Yun Gao,Wenli Wang,Li Su,Beixing Li,Wei Mu,Weili Yu
Bupirimate is widely used as a highly active systemic fungicide. However, the frequent and heavy use of bupirimate has led to pesticide residues in crops that threaten human health and food safety. At present, there is limited research on the detection of ethirimol, which is the metabolite of bupirimate. This study established an ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method to simultaneously detect bupirimate and ethirimol residues based on QuEChERS pretreatment. The average recoveries of bupirimate and ethirimol in cucumber were between 95.2 and 98.7%, respectively, with relative standard deviations (RSDs) of 0.92–5.54% at fortified levels of 0.01, 0.1, and 5 mg L–1. The established method was used to determine the residues in field trials in 12 regions of China, and the final residues of bupirimate were all less than the maximum residue limit (MRL). Since the risk quotient (RQ) of bupirimate and ethirimol in cucumber was less than 1.3%, the dietary risk assessment indicated that bupirimate and ethirimol had a low long-term dietary risk to the general population in China. This study provides effective guidance on the proper use of bupirimate in cucumber fields and a reference for establishing the MRL of bupirimate in China.
研究领域:
植物保护
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食品安全
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分析化学
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PubMed
高影响因子
Food Science & Nutrition
·
2026
·Vol. 14
·期 4
·e71593
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IF 5
Diaodiao Yang,Jianwen Liu,Yang Song,Yajing Ma,Hongkang Zhu,Qingfeng Zhou,Maomao Zeng
Dietary exposure to both processing contaminants and natural toxins in fried foods poses a potential health risk, but analytical methods for their simultaneous monitoring are lacking. To address this gap, a rapid and efficient method based on QuEChERS extraction and UPLC–MS/MS detection was developed for the simultaneous determination of two β-carboline heterocyclic amines (harman and norharman) and seven mycotoxins (fumonisins B1, B2, B3 and aflatoxins B1, B2, G1, G2). The optimized extraction utilized a 30:20:50 (v/v/v) acetonitrile/methanol/water mixture. The method was rigorously validated, showing high sensitivity (LODs: 0.021–0.232 ng/g; LOQs: 0.100–0.587 ng/g), accuracy (recoveries: 80.4%–109.3%), and reliability. When applied to real samples, the method not only confirmed its practicality across different matrices but also revealed a critical finding: the co-occurrence of heterocyclic amines and mycotoxins, particularly in fried peanuts. This study provides an essential tool for integrated food safety surveillance and highlights the need for combined risk assessment of multiple contaminants.
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Analytical Methods
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2015
·Vol. 7
·期 19
·8418-8431
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IF 1.821
Mei Yang,Youning Ma,Wenjun Gui,Yiping Ren,Guonian Zhu,Yihua Liu
Endocrine-disrupting chemicals (EDCs) in the environment have adverse effects on humans and wildlife. A method based on ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for the determination of 26 EDCs (including five estrogens, eight androgens, three progestogens, six glucocorticoids, two mineralocorticoids and two thyroid hormones) in fish and water was developed. Various experimental parameters that could affect the extraction efficiencies were investigated in detail. The sample was extracted by a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method with 20 mL of acetonitrile (for fish) or 5 mL of ethyl acetate (for water), and then cleaned-up using an Oasis HLB SPE (solid-phase extraction) cartridge. The analytes were quantified using an isotope-labelled internal standard and recoveries between 69.1% and 120.5% were obtained. The relative standard deviation of inter- and intra-day analyses for all the compounds was below 20%. The detection limits ranged from 0.01 to 0.98 ng mL−1 for water and 0.01 to 9.04 ng g−1 for fish. For real samples, progesterone and trenbolone were detected in zebrafish (Danio rerio) samples at 5.73 ± 0.21 and 7.45 ± 0.34 ng g−1, respectively. There was no target analyte detected in tap-water samples. The developed method would be useful for monitoring EDC abuse in fishery, potential EDC screening and risk assessment in aquatic toxicology.
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JOURNAL OF SEPARATION SCIENCE
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2026
·Vol. 49
·期 5
·e70448
·
IF 3.6
Tao Pei,Xueyun Wang,Jiye Hu
To control thrips in eggplant cultivation, a new pesticide formulation (9% emamectin benzoate·spinetoram microemulsion) is under registration in China. However, the residues of emamectin benzoate (EMB), spinetoram, and prime metabolites of spinetoram in eggplant remained unclear. In this study, field trials were performed in accordance with good agricultural practice across eight provinces of China. The pesticide formulation was sprayed once at 13.5 g a.i./ha, and the recommended pre-harvest interval was 7 days. For the simultaneous determination of EMB, spinetoram, and its metabolites in eggplant, a modified quick, easy, cheap, effective, rugged, and safe method combined with high-performance liquid chromatography tandem mass spectrometry was developed and validated. The combination of 25 mg of primary-secondary amine, 25 mg of Nano-ZrO 2 , and 5 mg of multi-walled carbon nanotubes was applied to purify the eggplant extracts. Method validation demonstrated excellent linearity ( r ≥ 0.9991), acceptable accuracy with recoveries of 82.7%–102.6%, precision (relative standard deviations ≤7.7%), sensitivity (limits of detection, 6.59 × 10 −5 –3.06 × 10 −3 ng; limits of quantification, 0.0025–0.01 mg/kg), and matrix effects (≤25.2%). When harvested after the recommended 7-day interval, the residues of EMB (<0.01 mg/kg) and spinetoram (≤0.025 mg/kg) in eggplant were lower than the maximum residue limits in China. The residues of metabolites N- formyl-XDE-175-J and N- demethyl-XDE-175-J in eggplant were lower than the limits of quantification (0.01 mg/kg). This study offers recommendations for the effective use of this pesticide formulation on eggplant.
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高影响因子
TALANTA
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2020
·
IF 5.339
Qingyi Wei,Ting Liu,Hongbin Pu,Da-Wen Sun
Acrylamide (AM), as one of the by-products produced by the Maillard reaction, has received increasing attention due to the potential risk of side effects in humans and other animals. In this study, a simple method was developed for AM quantitation by utilizing the fluorescence enhancement induced by the distance increase between functionalized carbon quantum dots modified by N-acryloxysuccinimide (NAS-CQDs) induced by AM polymerization. This fluorescent sensing approach allowed for detecting AM in a double-distilled water system in the range between 5 × 10 −3 and 1 × 10 −6 M with a low detection limit of 2.6 × 10 −7 M. Furthermore, a novel method for the pretreatment of white bread crust samples was developed based on QuECHERS method (Quick, Easy, Cheap, Effective, Rugged and Safe), and detecting range between 5 × 10 −4 and 5 × 10 −6 M, low detection limit of 8.1 × 10 −7 M, and satisfactory recoveries of 99.13–103.7% in spiked white bread crust samples were obtained by the present method, confirming its good applicability for AM determination in real food products.
研究领域:
食品科学
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分析化学
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纳米技术
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PubMed
高影响因子
JOURNAL OF HAZARDOUS MATERIALS
·
2025
·
IF 11.3
Ruidong Zhou,Xinyuan Zhang,Yupeng Wen,Wendi Huo,Yingchun Mu,Huan Liu,Chaoying Zhang,Jincheng Li
Multi-walled carbon nanotubes (MWCNTs) are known for their excellent purification properties in QuEChERS-based pesticide analysis, but their potential release and non-recyclability pose environmental and economic challenges. In this study, a novel strategy is proposed to immobilize MWCNTs with chitosan, forming the MWCNTs@chitosan composite, which enables the recyclability of MWCNTs. This composite was employed in a one-step pressure filtration purification method to simultaneously purify extracts of 49 pesticides from aquatic products. Coupled with HPLC-MS/MS, an optimized QuEChERS method was successfully validated for the determination of 49 pesticides. The MWCNTs@chitosan composite demonstrated excellent clean-up capability, effectively removing interfering substances from crude extracts while maintaining recoveries of 71.2–119.4 % and relative standard deviations (RSDs) below 20.0 %. These results demonstrate the composite’s suitability as a QuEChERS cleanup material, with potential applications in other complex matrices.
研究领域:
环境科学
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分析化学
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食品安全
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纳米技术
·
材料科学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
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2024
·
IF 8.5
Jiayu Chen,Liyuan Zhang,Runzhong Yu
A nucleic acid aptamer based thermally oxidized porous silicon/zinc oxide microarray chip was constructed for the detection of ochratoxin A. The hybrid chains formed by aptamer and complementary chains labeled with fluorescent groups and fluorescent burst groups were used as recognition molecules, and the detection of toxins was accomplished on the chip by the principle of fluorescence signal burst and recovery. The modified QuEChERS method was used for sample pretreatment and the performance of the method was evaluated. The results showed that the linear range was 0.02 ∼ 200 ng/kg with the detection limit of 0.0196 ng/kg under the optimal detection conditions. The method was applied to different cereals with the recoveries of 90.30 ∼ 111.69 %. The developed microarray chip has the advantages of being cost-effective, easy to prepare, sensitive and specific, and can provide a new method for the detection of other toxins.
研究领域:
分析化学
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食品科学
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毒理学
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生物传感器
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PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2026
·
IF 5.2
Rongqiao Chen,Wei Chen,Ming Liang,Junpeng Hu,Ruifang Fan,Guoshan He,Yanping Xian
Liquid crystal monomers (LCMs) are emerging environmental contaminants with bioaccumulation potential and health risks. Chinese herbal medicines, susceptible to LCM uptake during cultivation or processing, represent a potential human exposure route. However, reliable methods for analyzing LCMs in these complex matrices are lacking. Herein, a modified QuEChERS method coupled with gas chromatography–tandem mass spectrometry (GC–MS) was developed for the determination of 10 LCMs in herbal medicines. Samples were extracted with dichloromethane and cleaned up using mixed sorbents (N-propyl ethylenediamine and octadecylsilane). The method showed excellent linearity (2.0–200.0 μg/L, r 2 > 0.999), with limits of detection and quantification of 0.5–2.0 μg/kg and 1.0–5.0 μg/kg, respectively. Mean recoveries across three spike levels in different matrices ranged from 75.0% to 112.9%, with relative standard deviations of 2.0–8.5% ( n = 6). In the analysis of 26 real herbal medicines samples, LCMs were detected in mulberry leaf and Salvia miltiorrhiza , indicating a detection frequency of 7.7% and potential contamination in herbal medicines. This reliable and practical method is suitable for routine monitoring of LCM residues in various herbal products.
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ACS Omega
·
2022
·
IF 4.132
Lei Zhu,Li Liu,Le Du,Jingmei Hao,Jianhua Ma,Jun Zhu,Wenjing Gong
A rapid, accurate, and selective analytical method to simultaneously quantify 13 anticoagulant rodenticides in animal biological samples was developed using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) coupled with electrospray ionization (ESI) in negative mode. Samples were extracted and purified based on a modified QuEChERS (quick, easy, cheap, effective, rugged, safe) sample preparation technique. The sample pH and the type of extraction solvent and cleanup sorbent used to estimate the procedure’s effectiveness were optimized. To improve the matrix effects and obtain acceptable recoveries for 13 rodenticides, 0.1 mL/g biological sample and 1 mL acetonitrile (or acetonitrile: EtOAc = 1:1/(v:v)) extraction followed by Florisil/HC-C18/anhydrous Na2SO4 (NaCl) cleanup under alkaline conditions was fully validated and shown to be selective, precise, accurate, and linear in the range from 1 to 100 ng/mL (g). The mean recoveries were between 52.78 and 110.69%, while the limits of detection and quantification ranged from 0.05 to 0.5 and 0.1–1 ng/mL (μg/kg), respectively. Ideal soft matrix effects (≤20%) were observed for the vast majority of rodenticides (>95%) showing either suppression or enhancement. This method meets international criteria and is capable of simultaneously identifying and quantifying anticoagulant rodenticides in animal blood and tissues and can be suitable for the detection of poisoning cases in the field of forensic or public health.
研究领域:
分析化学
·
毒理学
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法医学
·
公共卫生
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DOI
PubMed
高影响因子
ANALYTICAL SCIENCES
·
2026
·
IF 2
Lu Chang,Ma Wei-bo,Wang Jun,Duan Ding-ding,Chen Zhi-zhou,Ma Yan-li
Accurate quantification of pesticide residues is critical to ensure the quality and safety of Rhizoma Polygonati , a well-recognized medicine-food homologous herb widely applied in functional food development. Strong matrix interference in gas chromatography-tandem mass spectrometry (GC-MS) detection and notable quantitative bias are frequently induced by the abundant pigments, polysaccharides, saponins and endogenous components in the herbal matrix. Conventional PSA and C 18 adsorbents in standard QuEChERS protocols exhibit restricted purification capacity for this complex matrix, while most documented magnetic carbon-based adsorbents demand tedious pre-synthesis procedures that may block the active adsorption sites of nanomaterials. A modified QuEChERS-GC-MS method coupled with dynamic in-situ assembly strategy was established for 12 pesticide residues in Rhizoma Polygonati . Without pre-synthesis of any composites, in-situ functional synergy between NH 2 -SWCNTs and magnetic Fe 3 O 4 nanoparticles was achieved during the dispersive solid-phase extraction (d-SPE) step. Superior purification performance to conventional adsorbents was obtained by this system, with the matrix effect range of target pesticides narrowed from -31.4%−64.3% to -25.3%−36.7%. Favorable linearity ( R ≥ 0.9990), acceptable spiked recoveries (86.2%–106.5%) and stable precision (RSD ≤ 15.20%) were validated through systematic method validation, providing a feasible and robust analytical protocol for pesticide residue monitoring in Rhizoma Polygonati and other complex herbal matrices. Graphical abstract
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危险品化学品经营许可证（带存储）