INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY
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2024
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IF 2.3
Fengqin Tu,Qing Xu,Shu Wang,Huiwen Fang,Zhe Chen,Hui Yu,Jing Hou,Tingjuan Xia,Yuepeng Lu,Jinglei Zhao,Yong Yang,Xiaoming Jiang
In this study, a rapid, effective method based on QuEChERS was optimised and validated for determination of perfluorooctanoic acid (PFOA) and perfluorooctane sulphonic acid (PFOS) in edible vegetable oils by high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). Samples were simply vortex extracted with methanol containing 1% ammonia solution and purified through C18, PSA and GCB, followed by determination with HPLC-MS/MS. The detection parameters, including the mobile phase composition, the chromatographic column, as well as the sample preparation conditions, such as the choice of extraction solvents and the dosage of C18, PSA and GCB cleanup agents were optimised. The quantification of target compounds was carried out using stable isotope internal standards to compensate for any matrix effect during the electrospray ionisation process in the mass spectrometry. The developed method has demonstrated commendable accuracy, with recovery percentages ranging from 93.76% to 108.96%, and exhibits excellent precision, as indicated by relative standard deviation not exceeding 20%. Furthermore, the method has been validated for its selectivity, linearity of response, and sensitivity. The proposed method is beneficial for gathering residue data on PFOA and PFOS, allowing for the evaluation of their contamination levels in edible vegetable oils available in the Chinese market and providing scientific backing for regulatory supervision.
研究领域:
分析化学
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食品安全
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环境科学
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产品关联
DOI
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2014
·Vol. 406
·期 18
·4563-4569
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IF 3.578
Xie Qilong,Liu Shuhui,Fan Yingying,Sun Jianzhi,Zhang Xiaoke
A selective and low organic-solvent-consuming method of sample preparation combined with high-performance liquid chromatography with diode-array detection is introduced for analysis of phthalic acid esters in edible oils. Sample treatment involves initial liquid–liquid partitioning with acetonitrile, then QuEChERS cleanup by dispersive solid-phase extraction with primary secondary amine as sorbent. Preconcentration of the analytes is performed by ionic-liquid-based dispersive liquid–liquid microextraction, with the cleaned-up extract as disperser solvent and 1-hexyl-3-methylimidazolium hexafluorophosphate as extraction solvent. Under the optimized conditions, correlation coefficients ( r ) were 0.998–0.999 and standard errors ( S
y / x
) were 2.67–3.37 × 10 3 for calibration curves in the range 50–1000 ng g −1 . Detection limits, at a signal-to-noise ratio of 3, ranged from 6 to 9 ng g −1 . Intra-day and inter-day repeatability, expressed as relative standard deviation, were in the ranges 1.0–6.9 % and 2.4–9.4 %, respectively. Recovery varied between 84 % and 106 %. The developed method was successfully used for analysis of the analytes in 28 edible oils. The dibutyl phthalate content of four of the 28 samples (14 %) exceeded the specific migration limit established by domestic and international regulations.
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研究领域:
分析化学
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食品安全
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2022
·
IF 4.52
Ming Yang,Jun Yi,Cong Wei,Yuepeng Lu,Yong Yang,Zong Yang,Liuqin Zhao,Xiaoming Jiang,Fengqin Tu
In this study, a method of ultrasonic assisted derivatization combined with improved QuEChERS scheme and high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was developed for the analysis of nitrofuran metabolite residues in honey samples. The optimized conditions such as ultrasonic assisted derivatization conditions, extraction methods and purification materials quantitatively obtained by matrix standard curve external standard method had finally been proved to be effective in the determination of nitrofuran metabolite residues in honey samples. In order to make the results more accurate, the matrix matched standard for isotope-labeled internal standard method was used for methodological verification. The concentration of all target substances ranged from were 0.25–20 ng/mL, with good linearity, and the correlation coefficient were 0.9999. The LOD and LOQ of the target analyte were 0.15 and 0.5 μg/kg respectively. The average recoveries of the three standards were between 1.89 % and 107.9 %. The recoveries of inter-day and intra-day tests were 96.0–100.2 % and 93.2–98.7 % respectively. The precisions of inter-day(n = 6) and intra-day(n = 6) analysis were 3.56–5.29 % and 3.09–5.13 % respectively. 85 honey samples obtained from the market were analyzed by our optimized method, of which 4 SEM and 1 AOZ were detected in 5 samples.
研究领域:
分析化学
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食品安全
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2025
·
IF 4
Chenguang Zhou,Peng Xiao,Huiling Huang,Jiangqi Huang,Jinyuan Sun,Siyao Liu
A novel Sin-QuEChERS cleanup method was developed for multi-pesticide residue analysis in Codonopsis radix by introducing a compressible composite adsorbent—isoreticular metal-organic framework-3 (IRMOF-3)/multi-walled carbon nanotubes (MWCNTs)-functionalized melamine sponge (MOF/MT@MeS). This innovative material enables one-step matrix cleanup through immersion and physical squeezing, eliminating the need for centrifugation and multiple sorbents required in conventional QuEChERS method. The covalent integration of amino-functionalized IRMOF-3 and MWCNTs exploits synergistic hydrogen bonding and π–π interactions for efficient purification. The composite significantly suppressed matrix effects (–12.7 to 17.4% vs –30.9 to 32.8%). Compared to traditional adsorbent materials, the composite yielded more consistent pesticide recoveries (90.4–117.9% vs 83.7–123.4%). The validated method exhibited excellent linearity (R², 0.9934–0.9991), high sensitivity (detection limits 0.54–8.33 μg/kg), and satisfactory accuracy with recoveries of 72.4–111.9% and RSD ≤14.1%. This work establishes functionalized sponge-based adsorbents as an efficient, rapid, and reliable alternative for pesticide monitoring in complex botanical matrices.
研究领域:
分析化学
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药物代谢
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食品安全
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中药质量控制
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环境污染物检测
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
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2020
·Vol. 59
·期 3
·269-279
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IF 1.28
Qian Bing,He Yan,Zhao Jing,Peng LiXu,Han BingJun
A sensitive, confirmatory ultra-high performance liquid chromatography–tandem mass spectrometry based on modified QuEChERS was developed and validated to detect five organotin compounds (tributyltin chloride (TBT), triphenyltin chloride (TPT), trimethyltin chloride (TMT), azocyclotin and cyhexatin) in classical tropical fruits (mango, pineapple and banana). Fruits samples were ultrasonically extracted with methanol and subsequently purified by graphitized carbon black adsorbents. Five organotins were separated on a C18 column with the mobile phase of a mixture of methanol and 0.1% (v/v) aqueous formic acid, and detected by MS/MS under multiple reaction monitoring mode. The developed method was validated in terms of linearity, limit of detection (LOD), recovery and precision. Results were linear in their corresponding concentration ranges, with coefficients of determination (r) bigger than 0.999. The average LODs (S/N = 3) of the method for TBT, TPT, TMT, azocyclotin and cyhexatin were 1.3, 3.5, 3.2, 5.1 and 1.7 μg/kg, respectively. The average recoveries (n = 5) at three spiked levels (0.01, 0.1 and 0.2 mg/kg) ranged from 69 to 103% with relative standard deviations of 2.1–11.9%. The method is simple, effective, accurate and non-derivatized, and meets the routine monitoring requirements for trace organotins in tropical fruits.
研究领域:
分析化学
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食品安全
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF ENVIRONMENTAL SCIENCE AND HEALTH PART B-PESTICIDES FOOD CONTAMINANTS AND AGRICULTURAL WASTES
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2021
·
IF 1.99
Zhongbei Zhang,Kai Ding,Zhou Lu,Nan Fang,Bo Wang,Zhiguang Hou,Zhongbin Lu
In the present study, an analytical method that combined a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method and high-performance liquid chromatography coupled with tandem mass spectrometry was developed to determine trifluorocide in fresh and dried ginseng roots, plants (stems and leaves), and soil. At three spiked levels (0.01, 0.1, and 1.0 mg kg−1), the mean recoveries (n = 15) of trifluorocide from fresh and dried ginseng roots, plants, and soil were in the range of 95.6 − 109.7%, with relative standard deviations less than 10.0%. The limits of quantitation of different matrices were determined to be 0.01 mg kg−1. Dissipation and residue study of trifluorocide was conducted in ginseng cultivation ecosystems in Northeast China. The t1/2 (half-life) of trifluorocide in ginseng fresh roots, plants, and soil were 8.3–13.1 days, 7.4–10.9 days, and 8.8–10.6 days, respectively. The terminal residues of trifluorocide in ginseng fresh roots were less than 0.01 mg kg−1 after 35 days of trifluorocide application. This study could be beneficial in residue analysis and assist in the scientific application of trifluorocide during ginseng cultivation.
研究领域:
植物保护
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环境科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
Food Analytical Methods
·
2020
·Vol. 13
·期 3
·823-832
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IF 2.667
Ye Xuemin,Shao Hua,Zhou Ting,Xu Jiahui,Cao Xiaoji,Mo Weimin
A modified QuEChERS protocol with a nitrogen-doped graphitized carbon derived from dicyandiamide sludge as a cleanup sorbent has been developed to determine 20 organochlorine pesticides in tomatoes using gas chromatography coupled to a triple-quadrupole mass analyzer. Compared with traditional QuEChERS adsorbents, N-doped graphitized carbon exhibited higher recoveries toward the target pesticides in tomatoes. And the modified protocol exhibited the advantages of environmental-friendly and low-cost. The use of dicyandiamide sludge to produce NGB as an adsorbent for QuEChERS opened up a new field for the comprehensive utilization of dicyandiamide waste. Under the optimum conditions, the modified method provided excellent linearity with correlation coefficient higher than 0.9980 and low limits of detection ranging from 0.001 to 0.1 μg/kg. The mean recoveries of the majority of pesticides in tomatoes ranged from 71.2 to 95.3% with relative standard deviation lower than 20%. Thus, the proposed protocol could be considered a good alternative for traditional QuEChERS method for pesticide analysis in agricultural vegetables.
研究领域:
食品科学
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环境科学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2025
·
IF 4.6
Chunlan He,Yunxi Tang,Shiqi Chen,Siyu Huang,Youming Xiong,Yamin Bai,Jingbing Xu,Yi Zhong,Hong Cheng,Lei Wang,Zhong Chen,Changjun Hou
Per- and polyfluoroalkyl substances (PFASs) have been widely detected in animal samples. But the fats, indispensable tissue in animals, can seriously hinder the PFASs extraction due to their nature of complex, unbreakable, and concretionary. To address this, a new sample preparation method, combining the advantages of ASE and QuEChERS, is proposed. Firstly, the extraction conditions of new method are optimized as co-solvent of MeCN+H 2 O, temperature of 100 °C, and time of 30 min. The MeCN performs better than MeOH because the MeOH will bring some impurities (phospholipids). The H 2 O under high temperature plays important dual functions of digestion and organic solvent. The exothermic reaction of MgSO 4 also enhance the PFASs extraction. Next, 15 animal samples are screened by both the new ASE+QuEChERS and traditional QuEChERS. The lower and upper limits of quantitation are 0.25 ng g −1 and 25.00 ng g −1 , respectively. Nine PFASs are detected in five positive simples. The new method can improve the total concentration of PFASs by range from 6 % to 64 %. Lastly, both the new ASE+QuEChERS and traditional QuEChERS methods are validated based on 10 relevant food simples. This study provides a simple, efficient and practical method for extraction of PFASs from animal 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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毒理学
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产品关联
DOI
高影响因子
MOLECULES
·
2022
·Vol. 27
·期 17
·5737
·
IF 4.927
Siwei Wang,Xiaonan Wang,Qiang He,Haidan Lin,Hong Chang,Haibin Sun,Yanping Liu
This study established a QuEChERS high-performance liquid chromatography/tandem triple-quadrupole mass spectrometry method for determining azoxystrobin, pyraclostrobin, picoxystrobin, difenoconazole, chlorantraniliprole, imidacloprid, and cyantraniliprole and its metabolite (IN-J9Z38) in litchi and longan, and applied this method to the real samples. The residues in samples were extracted with acetonitrile and purified with nano-ZrO2, C18, and PSA. The samples were then detected with multireactive ion monitoring and electrospray ionization in the positive ion mode and quantified using the external matrix-matched standard method. The results showed good linearities for the eight analytes in the range of 1–100 μg/L, with correlation coefficients (r2) of >0.99. The limit of quantification was 1–10 μg/kg, and the limit of detection was 0.3–3 μg/kg. Average recovery from litchi and longan was 81–99%, with the relative standard deviation of 3.5–8.4% at fortified concentrations of 1, 10, and 100 μg/kg. The developed method is simple, rapid, efficient, and sensitive. It allowed the rapid screening, monitoring, and confirming of the aforementioned seven pesticides and a metabolite in litchi and longan.Keywords:QuEChERS;HPLC-MS/MS;litchi and longan;pesticide and metabolite;residue
研究领域:
分析化学
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食品安全
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植物保护
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2022
·Vol. 27
·期 5
·1681
·
IF 4.927
Yaping Gan,Yan Zhu
Since the quality and safety of food highly depend on its preservation and protection, the use of food packaging materials increases the risk of chemical contamination of the packaged food by migration. Herein, we focused on antioxidants, photoinitiators, UV absorbers and plasticizers which are extensive additives used in food packaging materials. In the present study, a rapid, simple, green and reliable method was developed and validated for the determination of twelve chemical additives in edible vegetable oils using SFC together with a modified QuEChERS procedure. Under the optimum conditions, twelve additives were separated within 10 min, and the consumption of the organic solvent was significantly reduced, which improved the environmentally friendliness. The performance of the developed method was evaluated. Good linearity (r > 0.999) was obtained in the range of 0.20–20.0 µg/mL and 0.50–20.0 µg/mL, respectively. The limits of detection and limits of quantification of the twelve additives in vegetable oils were 0.05–0.15 µg/mL and 0.15–0.50 µg/mL, respectively. Recoveries of all the chemical additives for the spiked samples were between 60.9% and 106.4%, with relative standard deviations (RSD) lower than 9.9%. The results demonstrated that the proposed method was efficient, reliable and robust for the routine analysis of additives in edible vegetable oils and can be an alternative to the multi-residue analysis of chemical additives for other packaged foods.Keywords:antioxidants;photoinitiators;UV absorbers;plasticizers;edible vegetable oils;QuEChERS;supercritical fluid chromatography
研究领域:
食品安全
·
分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Mantang Chen,Li Chen,Lining Pan,Ruihong Liu,Junwei Guo,Meijuan Fan,Xiaoyu Wang,Huimin Liu,Shaofeng Liu
Magnetic carbon composite (Fe 3 O 4 @C) was synthesized and applied as a reversed-dispersive solid-phase extraction sorbent for the simultaneous analysis of 40 pesticide residues in tobacco by ultrahigh-performance liquid chromatography coupled to quadrupole time-of-fight mass spectrometry. Compared to the traditional QuEChERS method, the optimized Fe 3 O 4 @C simplified clean-up process and exhibited better clean-up capability than conventional sorbents. The pesticides were qualitatively identified by accurate mass of protonated molecules, fragment ions, isotopic peak clusters, and retention time, and quantitatively determined by matrix-matched external standard method. Good linearity of the proposed method was obtained with R value greater than 0.997 for all target pesticides at concentration levels of 2–200 µg/L. The limit of detection ranged from 0.14 to 2.67 µg/kg. The recoveries and relative standard deviations of all target pesticides at three spiked concentrations of 20, 50 and 200 µg/kg were in the ranges of 80.8%–113.3% and 0.6%–16.3%, respectively. Compared with the reported methods for the analysis of multiple pesticide residues in tobacco, the proposed method has the advantages of simple to operate, high clean-up ability and less time-consuming in clean-up process.
研究领域:
分析化学
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烟草科学
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产品关联
DOI
PubMed
高影响因子
Frontiers in Environmental Science
·
2022
·
IF 5.411
Wang Siwei,Sun Haibin,Liu Yanping,Wang Xiaonan,Chang Hong
A modified-QuEChERS method to determine kresoxim-methyl in banana and soil was developed and validated via high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS). The dissipation behavior, residue distribution, and risk assessment of kresoxim-methyl in banana were further investigated based on this method. The dissipation behavior of kresoxim-methyl in banana and soil was described by using first-order kinetics and its half-life, 4.8–5.7 days and 5.5–6.5 days, respectively. The concentrations of kresoxim-methyl were 0.03–0.08 mg kg−1, 0.06–0.17 mg kg−1, and <0.01 mg kg−1 for a whole banana, peel, and pulp, respectively, on the basis of spraying three times the recommended dosage and pre-harvest interval (PHI, 42 days). The results showed that the risk quotient of kresoxim-methyl in banana to people exhibited an acceptable low dietary risk. This current study could help in guiding the scientific and proper usage of this formulation.
研究领域:
农业化学
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食品科学
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环境科学
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产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）