MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Shengji Lv,Shaoying Liu,Caili Zang,Bin Zhou,Xinglong Wang,Yuan Yao,Ming Xue,Ren Ren,Quan Jin
Pesticide pollution poses significant risks to human health, ecosystem, and biodiversity. Among agro-products, leafy vegetables exhibited particularly severe pesticide residue due to their short harvest periods and large leaf surfaces. However, investigations on multiresidues in high-risk leafy vegetables based on Chinese dietary habits were still limited. In this study, we developed a weak basic citrate-buffered QuEChERS method for the simultaneous extraction of 43 pesticides in bok choy, celery, Chinese chive and cilantro. Coupled with the high-throughput UPLC-MS/MS technique, this method achieved LODs ranging from 0.1–3.0 μg/kg and LOQs ranging from 0.4–10.0 μg/kg for the four matrices with high sensitivity. The recovery experiments on blank samples indicated that the method recoveries were in the range of 76.2 %–116.3 %, with RSDs less than 12.1 %. The developed method provided a highly accurate and precise technical approach for the analyses of high-risk leafy vegetables. Furthermore, 211 vegetables were collected from markets in Hangzhou from 2021 to 2023. The total detection frequency was 92.9 %, and high detection frequencies for pesticides such as acetamiprid, carbendazim, clothianidin, dimethomorph, dinotefuran, imidacloprid, propiconazole, pyraclostrobin, and thiamethoxam. The distribution of pesticides in different vegetables varied significantly due to factors such as application amount and plant absorption, providing valuable insights for implementing targeted detection and regulatory interventions. The mixed use of multiple pesticides in cilantro was observed. Combined use of pesticides such as tebuconazole, difenoconazole, and propiconazole (all belonged to sterol demethylation inhibitors), might lead to pathogen resistance. In summary, the frequently detected pesticides in the four leafy vegetables presented acceptable dietary risks, with hazard quotients ranging from 0.005 % to 3.634 %.
研究领域:
食品安全
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分析化学
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环境科学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2026
·
IF 2.5
Peiqi Sun,Fei Hang,Jiayang Wang,Yuanye Jiang,Lingyun Pan,Cheng Hu
Sphingosine (SP), dihydro-sphingosine (DSP), and sphingosine 1-phosphate (S1P) are integral metabolites in the sphingolipid pathway. They exhibit intricate and diverse functions in the development of metabolic-associated fatty liver disease (MAFLD). In this study, we developed a highly sensitive and specific analytical approach for the concurrent quantification of these three sphingolipids in human plasma, utilizing ultra-high-performance liquid chromatography (UPLC), in conjunction with tandem mass spectrometry (MS/MS). A stripped biological matrix was generated through optimized activated‑carbon treatment to facilitate more accurate calibration. The sample preparation involved a straightforward protein precipitation method using methanol, followed by concentrating the supernatant and reconstituting it prior to injection. Detection was executed in the multiple reaction monitoring mode with a triple quadrupole mass spectrometer. The chromatographic separation was achieved on a Waters ACQUITY UPLC HSS C 18 column employing gradient elution. D-erythro-sphingosine-d 7 served as the internal standard. The newly established method conformed to recognized standards for selectivity, linearity, accuracy, precision, recovery, matrix effects, and stability. This technique was effectively applied to quantify the three sphingolipid metabolites in plasma samples collected from patients diagnosed with MAFLD ( n = 30), and healthy controls (n = 30). Analysis of the data revealed significant differences between the groups, with the levels of SP, DSP, and S1P considerably elevated in MAFLD patients compared to healthy subjects.
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高影响因子
Environmental Science-Water Research & Technology
·
2023
·Vol. 9
·期 4
·1231-1237
·
IF 5
Run Zhou,Zhifei Xu,Yukang Wu,Li Yang,Xiuzhu Li,Yuanhua Meng,Pengfei Zhu,Lingcan Kong,Xinliang Ding
Human exposure to disinfection by-products (DBPs) primarily occurs through the consumption of drinking water. Haloacetamides (HAcAms) are an emerging class of nitrogenous DBPs with higher levels of cytotoxicity and genotoxicity compared to those of regulated DBPs. Detecting ultra-trace levels of HAcAms in drinking water remains challenging despite the availability of multiple detection methods. This paper reports the first use of ultra-performance liquid chromatography–mass spectrometry/mass spectrometry (UPLC-MS/MS) to quantify 13 HAcAms in drinking water without pretreatment. Results from the analysis of water samples collected from four cities in East China showed total HAcAm concentrations of 0.21–6.12 μg L−1, which were comparable to previously reported data from other countries. Further, 11 out of 13 HAcAms were detected in 60 water samples, with diHAcAms being the predominant subclass. DCAcAm and BCAcAm were the primary HAcAms targeted for detection and two Iodo-HAcAms were detected. The average total HAcAm concentration in water samples disinfected with chloramine was significantly higher than that in water samples disinfected with chlorine. Additionally, the total HAcAm concentrations in water samples from a treatment plant (WTP) using the ozone-biological activated carbon (ozone-BAC) process were lower than those in water samples from WTPs that did not use this treatment process. The results of this study have significant implications for monitoring water quality and protecting human health.
研究领域:
环境科学
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公共卫生
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分析化学
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DOI
高影响因子
Journal of Materials Chemistry B
·
2021
·Vol. 9
·期 14
·3192-3199
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IF 6.331
Yuanchen Liu,Yujian Liu,Zhiming Liu,Jonathan P. Hill,Azhar Alowasheeir,Zhigang Xu,Xingtao Xu,Yusuke Yamauchi
Traditional analysis methods are susceptible to interference caused by the complexity of sample matrices, and detector surface fouling arising from nonspecific adsorption of microorganisms (in biological samples) which leads in particular to a gradual loss of sensitivity. Imprinted materials can be used to effectively reduce interference originating in the matrices. However, the poor reproducibility and multicomponent quantification of trace antibiotics represent significant challenges to the detection process. Meanwhile, the high biological risk presented by bacterial antibiotic immunity and the persistence of antibiotics in foodstuffs, especially meat, both caused by the overuse of sulfonamide antibiotics, remain urgent issues. Here, we present the first example of a method for the accurate quantification of trace sulfa antibiotics (SAs) based on multi-template imprinted polymers (MMIPs). Levels of multiple SAs have been simultaneously successfully quantified by applying MMIP extraction coupled with UPLC-MS/MS analysis. This method shows excellent linearity of detection in the range of 0.1–500 μg L−1, and ultrasensitivity with low limits of detection of 0.03 μg L−1. The maximum SA residue recovered from sample tissues by using MMIPs was 5.48 μg g−1. MMIP-coupled UPLC-MS/MS quantification of SAs is an accurate and repeatable method for the monitoring of SA accumulation in mouse tissue samples. It also provides an effective strategy for the tracking and quantification of drugs in other biological 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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DOI
PubMed
高影响因子
TALANTA
·
2024
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IF 5.6
Yifan Liu,Zihui Jin,Di Sun,Jiexin Zheng,Bo Xu,Tianyu Lan,Qiyang Zhao,Yue He,Jing Li,Yaohai Zhang,Yongliang Cui
Both rhoifolin and diosmin belong to flavonoids, which are widely present in citrus. Diosmin is not only used in the medical field in the world, but also used as a dietary supplement in the United States. Rhoifolin has a similar structure to diosmin and also exhibits antioxidant and anti-inflammatory properties. In this study, an anti-rhoifolin monoclonal antibody was prepared and an indirect competitive enzyme-linked immunosorbent assay (icELISA) method was established. The half-maximal inhibitory concentration (IC 50 ) of icELISA was determined to be 4.83 ng/mL, and the detection range was 0.97–33.87 ng/mL. The results of UPLC-MS/MS and icELISA generally demonstrate consistency. Moreover, by exploiting the cross-reactivity of the antibody, diosmin in tablets can be detected by icELISA. The results demonstrate that the developed method has good accuracy, reproducibility, and broad application prospects.
研究领域:
药理学
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分析化学
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免疫学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 6
·e4193
·
IF 1.688
Ping Guo,Jingjing Zhang,Xiaohui Chen,Longshan Zhao
A molecularly imprinted polymer was synthesized and applied as a sorbent in the solid-phase extraction device. The imprinted polymer was characterized by fourier-transform infrared spectroscopy and scanning electron microscope. The results revealed that imprinted polymer possess sensitive selectivity and reliable adsorption properties for five NSAIDs. The imprinted polymer was successfully applied to the pre-concentration for five NSAIDs in different water samples prior to UPLC-MS/MS. In the early studies, several factors were investigated, including pH adjustment, the kind of elution solvent and the volume of elution solvent. Finally, we found that the pH 5 and an aliquot of 2 mL methanol were suitable for the water samples. The limits of detection and limits of quantitation of five nonsteroidal anti-inflammatory drugs varied from 0.007 to 0.480 μg L −1 and 0.03 to 1.58 μg L −1 , respectively. The spiking recoveries of the target analytes were 50.33-127.64% at the levels of 0.2 μg L −1 , 2 μg L −1 and 5 μg L −1 . The precision and accuracy of this method showed a great increase compared with traditional solid-phase extraction. The developed method was successfully applied to extraction and analysis of NSAIDs in different water samples with satisfactory results which could help us better understand their environmental fate and risk to ecological health.
研究领域:
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
Journal of Functional Foods
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2017
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IF 3.144
Han Peng,Wenting Li,Hongyan Li,Zeyuan Deng,Bing Zhang
Both extractable (EPE) and non-extractable bound phenolic (BPE) in the seed coat and cotyledon of black bean were investigated in the present study. Their total phenolic contents (TPC) and antioxidant activities (DPPH, ABTS and FRAP) were evaluated, and the phytochemical compositions of EPE and BPE in both seed coat and cotyledon of black soybean were identified and quantified ( Glycinemax(L.) merr ) by UPLC-ESI-QTOF-MS/MS and UPLC-ESI-QqQ-MS/MS. In the present study, a total of 112 and 78 compounds were identified or tentatively characterized in the black soybean EPE and BPE, respectively, with the majority being phenolic acids and flavonoids. Seed coat contains more abundant phenolics than that of cotyledon in all fractions. In addition, our results indicated that acid hydrolysis is more thorough than alkaline hydrolysis in the extraction of bound phenolics of black soybean. Our study provides available information for non-extractable bound phenolic constituents and their distribution in the seed coat and cotyledon of black soybean.
研究领域:
植物化学
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食品科学
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DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2018
·
IF 2.831
Ni-hong Pang,Qian Liu,Xiang-ran Lu,Su-fen Yang,Dong-dong Lin,Guo-xin Hu
Enasidenib, an oral product for treating Acute Myeloid Leukemia, has been approved by FDA in Aug, 2017. In this study, we set up an ultra-performance liquid chromatography-mass spectrometry (UPLC-MS/MS) method for measuring Enasidenib and imatinib (internal standard, IS), simultaneously. Enasidenib and imatinib were separated on an ACQUITY UPLC BEH C 18 Column (2.1 mm × 50 mm, 1.7 μm, 132 Å). Mass detection was carried out by electrospray ionization in the position mode, and the multiple reaction monitoring transitions were m/z 474.23 → 456.17 and m/z 494.30 → 394.20 for Enasidenib and imatinib, respectively. Linearity (2 − 500 ng·mL −1 , R 2 > 0.999), precision and accuracy (RE < ± 15%), extraction recovery (≥ 96.69%), matrix effect (≥ 96.47%) and stability (RE < ± 10%) were validated which demonstrated the robustness of our method. This rapid, efficient and reliable UPLC-MS/MS method shows specificity and repeatability of Enasidenib in rat plasma and can be used in further pharmacokinetic studies.
研究领域:
药理学
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分析化学
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药物代谢动力学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2015
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IF 2.729
Wei Sun,Zhe-li Jiang,Lei Zhou,Rui-min Chen,Zhe Wang,Wan-shu Li,Shuo-min Jiang,Guo-xin Hu,Rui-jie Chen
A rapid, sensitive and selective ultra-performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS) was developed and validated for the determination and pharmacokinetic investigation of pirfenidone in rat plasma. Sample preparation was accomplished through a simple one-step deproteinization procedure with 0.2 mL of acetonitrile to a 0.1 mL plasma sample. Plasma samples were separated by UPLC on an Acquity UPLC BEH C18 column using a mobile phase consisting of acetonitrile-0.1% formic acid in water with gradient elution. The total run time was 3.0 min and the elution of pirfenidone was at 1.39 min. The detection was performed on a triple quadrupole tandem mass spectrometer in the multiple reaction-monitoring (MRM) mode using the respective transitions m / z 186.2 → 92.1 for pirfenidone and m / z 237.1 → 194.2 for carbamazepine (IS), respectively. The calibration curve was linear over the range of 5–2000 ng/mL with a lower limit of quantitation (LLOQ) of 5 ng/mL. Mean recovery of pirfenidone in plasma was in the range of 80.4–84.3%. Intra-day and inter-day precision were both <12.1%. This method was successfully applied in pharmacokinetic study after oral administration of 10.0 mg/kg pirfenidone in rats.
研究领域:
分析化学
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药理学
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DOI
PubMed
高影响因子
JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2020
·
IF 0.992
Hao Zhang,Juan Wei,Zongli Huo
A simple and rapid method employing ultra-high performance liquid chromatography tandem mass spectrometry has been developed for the direct determination of acrylic acid in tap water for the first time. The method worked on a ultra-high-performance liquid chromatography system and utilized the direct injection of 10 μL volumes. Aqueous samples were filtered with 0.22 μm membrane after diluting with the acetonitrile without any further pretreatment. The separation was accomplished by using a HILIC column with a gradient elution program. Acetonitrile and ammonium acetate solution (pH = 7) were applied in the method as the mobile phase. Acrylic acid- d3 was used as the internal standard in the quantification process. The method provided good recovery from 102.8% to 104.4%, good precision with intraday relative standard deviations in a range of 2.3% and 5.1%. The limit of quantification for the method was 45 μg/L. The possible structures of qualitative ion and quantitative ion of acrylic acid were proposed in this work with the help of the product ion spectra of acrylic acid and its corresponding isotopic standards. This study provided a reliable and quantitative method that could be used for daily monitoring of water quality.
研究领域:
分析化学
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环境科学
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DOI
高影响因子
INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
·
2022
·Vol. 23
·期 15
·8810
·
IF 6.208
Ting Xue,Wenqing Wang,Zhiyuan Yang,Fanjun Wang,Lei Yang,Jian Li,Hui Gan,Ruolan Gu,Zhuona Wu,Guifang Dou,Zhiyun Meng
The mole fraction of deacetylated monomeric units in chitosan (CS) molecules is referred to as CS’s degree of deacetylation (DD). In this study, 35 characteristic ions of CS were detected using liquid chromatography–electrospray ionization–mass spectrometry (LC–ESI–MS/MS). The relative response intensity of 35 characteristic ion pairs using a single charge in nine CS samples with varying DDs was analyzed using 30 analytical methods. There was a good linear relationship between the relative response intensity of the characteristic ion pairs determined using ultrahigh performance (UP) LC–MS/MS and the DD of CS. The UPLC–MS/MS method for determining the DD of CS was unaffected by the sample concentration. The detection instrument has a wide range of application parameters with different voltages, high temperatures, and gas flow conditions. This study established a detection method for the DD of CS with high sensitivity, fast analysis, accuracy, stability, and durability.Keywords:chitosan;degree of deacetylation determination;UPLC–MS/MS;relative response intensity of the characteristic peak
研究领域:
生物化学
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分析化学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2019
·
IF 5.399
Fei Xu,Feng Liu,Chaozhan Wang,Yinmao Wei
Magnetic solid-phase extraction (MSPE), using a new reversed-phase/weak anion exchange mix-mode mesoporous magnetic SiO 2 adsorbent, was assessed as an approach for reducing matrix effects in the analysis of six lipophilic marine biotoxins in shellfish using ultrahigh-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The adsorbent showed greater adsorption capacity and selectivity for the analytes and, thus, the MSPE microspheres reduced the matrix effects significantly in the subsequent analysis. In the UPLC-MS/MS analysis, precursor and product ions of the analytes were monitored quantitatively and qualitatively using multiple reaction monitoring and product ion confirmation modes. The proposed method exhibited a linear correlation of 0.9980–0.9991 in the working range for azaspiracids (2.0–200.0 ng/mL) and okadaic acid and its derivatives dinophysistoxins (4.0–200.0 ng/mL) with satisfactory recoveries (82.8–118.6%, RSD < 12%), lower LODs (0.4–1.0 μg/kg) and LOQs (1.0–4.0 μg/kg) than existing methods. In addition, consumption of the adsorbent was reduced, and the MSPE operation is simple and rapid relative to alternatives. These results suggest the proposed method has potential for use in the analysis of lipophilic marine biotoxins in shellfish samples.
研究领域:
分析化学
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海洋生物学
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毒理学
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DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）