Water
·
2024
·Vol. 16
·期 9
·1315
·
IF 3
Kan Li,Yiling Hu,Yuke Jiang,Xing Han,Xin Liu,Mingluo Du
The determination of illegal drugs and psychoactive substances in wastewater is increasingly being used to monitor the use of both by populations in specific areas. This article describes a method for the simultaneous determination of 78 illegal drugs and psychoactive substances in wastewater using direct-injection ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). This method includes the analysis of stimulants, opioids, antidepressants, antipsychotic drugs, anti-anxiety drugs, and hallucinogens. The method was validated in terms of the selectivity, calibration range, recovery, matrix effects, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ). The correlation coefficients were higher than 0.99 for all analytes, and the calibration range was from 0.2 to 500 ng/L. The LOD and LOQ of this method were 0.1–1 ng/L and 0.2–5 ng/L, respectively. The intra- and inter-day precisions were <9.3% and 11.4%, respectively, and the recovery ranged from 81.3% to 117.7%. The method was applied to real domestic wastewater collected from wastewater treatment plants, and the results showed that morphine, codeine, and ephedrine were detected in all samples. Some samples also contained other illegal drugs and psychoactive substances (such as etomidate, methamphetamine, ketamine, and tramadol). This indicates that the direct-injection UHPLC-MS/MS method can be used for the rapid determination of illegal drugs and psychoactive substances in wastewater.
研究领域:
环境科学
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分析化学
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毒理学
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产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2022
·
IF 9.231
Ying-yue Zhang,Mei-juan Zhao,Chun-yao Liu,Kai Ma,Tian-yu Liu,Fei Chen,Li-na Wu,De-jun Hu,Guang-ping Lv
Immunoassay-based techniques are important on-site screening tools for the detection of mycotoxins in cereals. This study aims to evaluate the trueness, precision, repeatability and cross-reactivity of commercially available test strips, ELISA kits and UHPLC-MS/MS on analyzing zearalenone, ochratoxin A, deoxynivalenol, T-2 toxin and fumonisin B 1 . The results showed that false negative rate (25.7 %–37.4 %) of all tested mycotoxins by test strips was higher than the false positive rate (0 %–31.0 %). The repeatability of ELISA kits at the declared LOD dispersed from −85.7 % to +98.4 %. ELISA kits were more accurate at 50 % of the maximum residue limit (MRL) of mycotoxins than 150 % and 200 %. All the tested deoxynivalenol/zearalenone derivatives had cross-reactivity with different level, and sample matrix could reinforce this overestimation of target mycotoxin. This study emphasized that higher-quality antibody screening and more analytical performance investigations are need to address for on-site detection of mycotoxins in the future.
研究领域:
食品科学
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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 CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2016
·
IF 2.687
Zhi Sun,Lihua Zuo,Jian Kang,Lin Zhou,Mengmeng Jia,Zeyun Li,Zhiheng Yang,Xiaojian Zhang,Zhenfeng Zhu
A rapid, sensitive, selective and accurate ultra high performance liquid chromatography with tandem mass spectrometry (UHPLC–MS/MS) method was developed and validated for the quantitation of prucalopride in rat plasma using carbamazepine as an internal standard (IS). Separation was achieved on a Waters ACQUITY UHPLC ® HSS C 18 column (2.1 mm × 50 mm, 1.8 μm) column with a gradient mobile phase consisting of acetonitrile–water (containing 0.1% formic acid) as mobile phase at a flow rate of 0.2 mL/min. Prucalopride and IS were monitored using positive electrospray triple quadrupole mass spectrometer (Waters Xevo TQD) via multiple reaction monitoring (MRM) mode. The monitored transitions were set at m / z 367.99 → 195.89 and m / z 236.97 → 194.04 for prucalopride and IS, respectively. The achieved lower limit of quantitation was 0.1 ng/mL. The validated method had an excellent linearity in the range of 0.1–100 ng/mL (r > 0.996). The intra- and inter-day precisions were both ≤ 7.8% for prucalopride and IS, and the average intra- and inter-day accuracies ranged from −3.0% to 8.5%. Extraction recoveries at three levels QC concentrations were in the range of 90.0–110.0% for prucalopride and 99.6% for IS. Matrix effects were found to be acceptable. The validated assay was successfully applied to a pharmacokinetic study of prucalopride following oral administration of 0.25, 0.5, 1.0 mg/kg to female and male rats respectively.
研究领域:
分析化学
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药物代谢动力学
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医学
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DOI
高影响因子
MOLECULES
·
2018
·Vol. 23
·期 8
·1926
·
IF 3.098
Bo Zhang,Xia Chen,Shun-Yu Han,Min Li,Teng-Zhen Ma,Wen-Jun Sheng,Xia Zhu
The aim of this study is to develop and validate an improved analytical method for the simultaneous quantification of 20 types of mycotoxins in grapes and wines. In this research, the optimization of tandem mass spectrometer (MS/MS) parameter, ultra-high pressure liquid chromatography (UHPLC) separation, and QuEChERS procedure, which includes wine/water ratio, the amount and type of salt, clean-up sorbent, were performed, and the whole separation of mycotoxins was accomplished within 7 min analyzing time. Under optimum conditions, recoveries ranged from 85.6% to 117.8%, while relative standard deviation (RSD) remained between 6.0% and 17.5%. The limit of detection (LOD, 0.06–10 μg/L) and the limit of quantification (LOQ, 0.18–30 μg/L) were lower than those permitted by legislation in food matrices, which demonstrated the high sensitivity and applicability of this efficient method. Finally, 36 grapes and 42 wine samples from the Hexi Corridor region were analyzed. Penicillic acid (PCA), mycophenolic acid (MPA), cyclopiazonic acid (CPA), fumonisin B1 (FB1) and zearalenone (ZEN) were detected in a small number of grape samples with lower concentrations between 0.10 μg/L and 81.26 μg/L. Meanwhile, ochratoxin A (OTA), aflatoxin B2 (AFB2), MPA, CPA, and ZEN were detected in some wine counterparts with concentrations ranged from 0.10 μg/L to 4.62 μg/L. However, the concentrations of the detected mycotoxins were much lower than the maximum legal limits set of other products.Keywords:QuEChERS;UHPLC–MS/MS;mycotoxins;grapes and wines;hexi corridor region
研究领域:
食品科学
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分析化学
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农业化学
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产品关联
DOI
PubMed
高影响因子
Food Chemistry-X
·
2024
·
IF 6.5
Guodong Mu,Sha Yan,Fei Pan,Haitao Xu,Xu Jing,Xiaofeng Xue
Beeswax, an FDA-approved component, has been extensively applied in feed, pharmaceutical, and food industries. The occurrence of neonicotinoid pesticides in beehive systems and their residues in beeswax have caused safety risks. Therefore, establishing a detection method for neonicotinoid pesticide residues in beeswax is crucial for ensuring its quality. The superhydrophobic property of beeswax makes it a challenge to develop suitable determination methods. In this work, we determined Proline and Oxalic acid as a suitable deep eutectic solvent (DES) to extract neonicotinoids from beeswax through theoretical design and verification tests. Systematic molecular dynamics simulations confirmed that hydrogen bonding and van der Waals forces facilitate the migration of neonicotinoid pesticides from beeswax into the DES. Performance analysis of the method revealed that the DES extraction combined with UHPLC-MS/MS approach exhibited excellent detection capabilities. It was applied to real beeswax sample analysis with the characteristics of simpleness, quickness, environmental friendliness, and high throughput.
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
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2020
·
IF 3.594
Kai Hu,Tiantian Pang,Yanmei Shi,Jiamin Cheng,Yanjie Huang
In this work, a facile strategy for the preparation of magnetic porous organic framework (Ni@POFs) was proposed by the reduction of Ni ions on its skeleton in situ. The properties of the material were confirmed by X-ray diffraction, vibrating sample magnetometer, infrared spectroscopy, transmission electron microscopy and scanning electron microscopy. The prepared Ni@POFs exhibits a strong magnetism and high extraction efficiency for targeted alkaloids. All the key factors that affect the extraction/desorption efficiency of the alkaloids onto the Ni@POFs material, such as sorbent amount, extraction time, sample pH and desorption condition, were investigated with the help of response surface methodology. In combination with magnetic solid phase extraction and ultra performance liquid chromatography-tandem mass spectrometry analysis, a novel method for the quantitative analysis of alkaloids in urine samples was proposed. The limits of detection and limits of quantitation for the eight alkaloids were found to be in the range of 0.9–6.0 and 3.0–20 pg mL −1 , respectively. The recoveries of spiked urine samples were in the range of 93.5–99.2% with RSDs less than 6.9%. The proposed method was successfully applied to analyze the metabolites in patient’s urine after the oral administration of berberine.
研究领域:
分析化学
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药理学
✓ 已验证
产品关联
DOI
高影响因子
MOLECULES
·
2019
·Vol. 24
·期 17
·3057
·
IF 3.06
Zili Guo,Bo Li,Jinping Gu,Peixi Zhu,Feng Su,Renren Bai,Xianrui Liang,Yuanyuan Xie
Orthosiphon stamineusBenth. (OS) is a traditional folk medicine for the treatment of kidney stones and other urinary tract diseases. In this study, a rapid and sensitive Ultra high-performance liquid chromatography (UHPLC)-MS/MS approach was established and validated for the simultaneous quantification of nine bioactive components in rat plasma. The nine components from OS extract detected in rat plasma were danshensu, protocatechuic acid, caffeic acid, rosmarinic acid, salvianolic acid A, salvianolic acid B, cichoric acid, sinensetin and eupatorin. After liquid-liquid extraction with ethyl acetate, the plasma samples were subjected to a triple quadrupole mass spectrometer employing electrospray ionization (ESI) technique and operating in multiple reaction monitoring (MRM) with both positive and negative ion modes. The standard curves showed good linear regression (r> 0.9915) over the concentration range for the nine analytes. The inter-day and intra-day precision and accuracy were found to be within 15% of the nominal concentration. The recovery and stability of nine compounds were all demonstrated to be within acceptable limits. The approach was successfully applied to investigate the pharmacokinetic analysis of the nine bioactive components after oral administration of OS extract in rats.Keywords:Orthosiphon stamineusBenth.;bioactive constituents;UHPLC-MS/MS;rat plasma;pharmacokinetic study
研究领域:
药理学
·
分析化学
·
传统医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2021
·
IF 3.205
Qianchun Zhang,Yongzhi Zhi,Linchun Bao,Yuguo Zheng,Xingyi Wang,Li Jiang,Yun Wu
Although parabens are useful due to their antiseptic properties, their widespread use has caused concerns regarding their potential toxicological effects. In this study, a novel magnetic solid-phase extraction combined with ultra-high-performance liquid chromatography-tandem mass spectrometry (MSPE-UHPLC-MS/MS) was developed, based on ordered magnetic mesoporous carbon (MMC), for paraben analysis. The MMC was prepared by soft-template synthesis, with a unique pore structure and a highly specific surface response, indicating potential as an excellent adsorbent. Several parameters affecting the paraben extraction efficiency were investigated and a novel method for paraben analysis in serum and urine samples using MSPE-UHPLCMS/MS was developed. The concentrations of methylparaben, ethylparaben, isopropylparaben, and propylparaben in these samples were 0.0380–4.36, 0.460–9.65, 0.0118–0.770, and 0.0363–0.641 μg/L, respectively, whereas isobutylparaben and butylparaben were not detected. Furthermore, satisfactory recoveries of 76.4–121% with relative standard deviations (n = 5) of 1.9–8.6% were obtained. Therefore, the developed MSPE-UHPLC-MS/MS method was efficient, highly sensitive, and reliable for analysing parabens in complex biological samples.
研究领域:
分析化学
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环境科学
·
毒理学
✓ 已验证
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Simin Zhuang,Dan Li,Yujun Liu,Chaomei Xiong
A rapid synthesis of carbamazepine (CBZ) magnetic molecularly imprinted polymer (MMIP) was proposed based on reflux precipitation polymerization method. The synthesis time for the formation of MIP coating on MMIP was shortened to less than 4 h. The characterization of MMIP demonstrates the successful synthesis of the imprinted layer. The adsorption selectivity of MMIP was systematically evaluated and showed fast selective recognition for CBZ. The MMIP based magnetic solid-phase extraction (MSPE) combined with UHPLC-MS/MS was developed, and its feasibility was validated in four complex matrices of environmental water, sediment, fish muscle and liver. It was successfully applied for the analysis of environmental water, sediment, and different fish tissues. Four environmental water samples from different sampling sites were found to contain CBZ at concentrations < LOD or LOQ, while the sediment samples collected at the same location did not contain CBZ. Two out of three wild snakeheads were found to contain CBZ, and the liver showed the highest residue. The study of drug exposed snakeheads indicate CBZ tends to accumulate in liver, followed by brain, heart and kidneys, and finally muscle and gills. The proposed method displays high potential for analyzing CBZ in complex environmental and biological samples.
研究领域:
分析化学
·
环境科学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF HAZARDOUS MATERIALS
·
2021
·
IF 10.588
Shuang Li,Jiping Ma,Gege Wu,Jinhua Li,Xiaoyan Wang,Lingxin Chen
A simple method based on magnetic solid-phase extraction (MSPE) was developed for the simultaneous extraction of eleven emerging aromatic disinfection byproducts (DBPs) in water samples coupled with ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS) determination. A magnetic covalent-organic framework (COF) material, namely, Fe 3 O 4 @TpBD, was facilely synthesized and fully characterized, followed by an MSPE process. Several important MSPE parameters, such as the magnetic ratio, Fe 3 O 4 @TpBD amount and sample pH, were systematically investigated. Under optimal conditions, the limits of detection and quantification of this COF-MSPE-UHPLC–MS/MS method were as low as 0.07–1.81 ng/L and 0.24–5.99 ng/L, respectively. Good precision was obtained with relative standard deviations (RSDs) of 1.3–10.9% (intraday) and 4.3–15.9% (interday). Furthermore, the validated method was proven applicable to real water samples; for example, the recoveries were 86.8–115.1% for the secondary effluent, and several DBPs in swimming pool water were detected. Notably, the MSPE process required only 7 min, ensuring that the DBPs were relatively stable during the whole analysis process and that Fe 3 O 4 @TpBD demonstrated excellent reusability. The COF-based MSPE method with simplicity, rapidity and efficiency provided an ideal sample pretreatment alternative to determine trace DBPs in complex matrices.
研究领域:
环境科学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2021
·
IF 3.205
Yue Zhang,Xiang-xiang Huo,Li-yuan Cheng,Meng-ying Chen,Lei Song,Ying-li Yu,Kun Zhou
β-Elemonic acid is one of the main active ingredients isolated from Boswellia carterii Birdw . which has been reported to exhibit potential anti-inflammatory and anti-cancer activities. There is few information about pharmacokinetics and tissue distribution of β-elemonic acid by now. In this study, an ultra-high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-MS/MS) method has been developed and validated to determine β-elemonic acid in rat plasma and various tissues after intragastric administration. Oleanolic acid was chosen as an internal standard (IS) and the plasma/tissue samples were pretreated with one-step liquid–liquid extraction. Chromatographic separation was accomplished on Eclipse Plus C18 analytical column (2.1 × 50 mm, 1.8 μm) utilizing a gradient mobile phase system consisting of water (with 0.1% ammonia-solution) and acetonitrile. β-Elemonic acid and IS were detected and quantified using negative electrospray ionization in multiple reaction monitoring (MRM) mode with transitions of m / z 453.3 → 423.5 for β-elemonic acid and m / z 455.3 → 407.6 for IS. β-Elemonic acid showed good linearity over the investigated concentration range (r > 0.9934) in rat plasma and tissue sample. The method was successfully applied for determination of β-elemonic acid in bio-samples. A bimodal phenomenon appeared in the plasma concentration–time curve of the β-elemonic acid. The highest tissue concentrations were found in the intestine including jejunum, ileum and colon.
研究领域:
药物分析
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药理学
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生物化学
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DOI
PubMed
高影响因子
CURRENT PHARMACEUTICAL DESIGN
·
2024
·Vol. 30
·期 32
·2574-2585
·
IF 2.6
Yuanjian Wang,Ruixun Wang,Huijia Wang,Ran Liu,Kaishun Bi,Qing Li
BackgroundEssential hypertension is a common clinical disease and a risk factor for cardiovascular and cerebrovascular diseases. Olmesartan medoxomil, amlodipine, and hydrochlorothiazide are commonly used antihypertensive drugs. The aim of this study was to establish a robust UPLC-MS/MS method for the simultaneous determination of olmesartan medoxomil, amlodipine, and hydrochlorothiazide in dog plasma. At the same time, the in vivo and in vitro release studies were conducted, and a preliminary in vitro-in vivo correlation (IVIVC) evaluation was performed.MethodsThe bioequivalence experiment was conducted with a double-crossed design. Three major components were extracted and analyzed by UHPLC-MS/MS. With the MRM scan, olmesartan and amlodipine were quantified by fragment conversion (m/z 447.10→190.10) and (m/z 408.95→294.00) under positive ESI mode, while hydrochlorothiazide was quantified with fragment conversion (m/z 295.90→268.90) under negative ESI mode. The in vitro release studies were performed using a USP paddle, and the dissolution medium was chosen from pH 6.0 to pH 6.8 according to the BCS classification of compounds. The IVIVC was calculated using the Wagner-Nelson equation.ResultsThe linear ranges of olmesartan, amlodipine, and hydrochlorothiazide in the plasma were 5.0-2500, 0.1-50, and 3.0-1500 ng/mL, respectively. All accuracies were within 3.8% of the target values, and the findings revealed that intra-day and inter-day accuracies were less than 12.1%. Moreover, the recoveries exceeded 88.3%, the matrix effect tests were positive, and the stability tests were positive. With the establishment of correlation, the distinguishable dissolution condition (pH 6.8) was selected as the predictable condition.ConclusionThe established method was suitable for the preclinical pharmacokinetic study of tripartite drugs with strong specificity and high sensitivity. Through the evaluation of IVIVC, the connection between in vivo and in vitro drug testing was initially established.
研究领域:
药理学
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分析化学
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临床医学
✓ 已验证
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）