Journal of Nanomaterials
·
2021
·
IF 2.986
Yangxu Luo,Juan Du,Huadi Xiao,Ling Zheng,Xuncai Chen,Ande Ma,Qizhi Luo
Accurate identification and quantification of methamphetamine (MA) and its related substances are essential for the investigation and fair trial of drug offenses. In this study, a modified LC-ESI-MS/MS method for the simultaneous determination of MA and its isomer N-isopropylbenzylamine (N-IBA) in forensic samples was developed and validated. Optimum chromatographic separation of the target analytes was achieved on an Agilent Poroshell 120 SB-C18 column ( mm, 2.7 μm) at 40°C with isocratic elution at the flow rate of 0.40 mL/min. The mobile phase was acetonitrile and 20 mM ammonium acetate solution containing 0.1% formic acid (80 : 20, ). Positive ESI-MS/MS detection was performed in multiple reaction monitoring (MRM) mode to identify and quantify the target analytes. Method validation showed excellent linearity in the range of 0.51 ng/mL~51 ng/mL for MA and N-IBA. The low limit of detection (LLOD) and low limit of quantification (LLOQ) reached 0.1 ng/mL and 0.3 ng/mL for both analytes. The method showed a satisfactory accuracy with an inter- and intraday-relative error (RE) <20%, and a precision of inter- and intraday relative standard deviation (RSD) less than 15%. The validated method was successfully applied in real forensic samples and resulted in the detection of MA and N-IBA in 8 suspected samples in drug cases that only deemed MA positive using our previous routine screening procedure, which avoided the misidentification of N-IBA as MA.
研究领域:
分析化学
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法医学
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产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
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2025
·
IF 5.1
Jie Wang,Yuan-Yuan Zhang,Dan Liu,Chen-Chun Zhong,Ya-Hui Hu,Fei Zhao,Hong-Li Guo,Feng Chen
The balance of oxalic acid in the body is intricately regulated. Importantly, elevated levels of oxalic acid in urine or blood have been linked to the progression of various diseases. There is strong interest in developing efficient methods to quantify oxalic acid in various bio-matrices like urine. However, due to its small molecular weight, high polarity, acidic nature, and endogenous properties, establishing an analysis method based on liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) for oxalic acid presents significant challenges, and such analysis methods that meet clinical needs are not widely available. Faced with the aforementioned challenging issues, in this study, we have discovered innovative strategies to improve the ionization, chromatographic separation, and enrichment of oxalic acid and its internal standard, leading to the successful LC-MS/MS method development and clinical application of the analysis method. These include: (1) simultaneous use of two low concentrations of electrolytes (NH 3 ·H 2 O and NH 4 Ac) in the mobile phase; (2) alkalinization of urine; (3) addition of 0.3 % NH 3 ·H 2 O to the internal standard oxalic acid-1,2- 13 C solution; (4) selection of ultrapure water (UPW) as an alternative matrix; (5) urine sample processing using an easy-to-use protein precipitation method. These measures have created a relatively homogeneous alkaline environment, addressing the issues in the ionization, chromatographic separation, and enrichment of oxalic acid and its internal standard. Of note, chromatographic separation of oxalic acid and oxalic acid-1,2- 13 C was achieved on the Waters Symmetry C18 column (4.6 mm × 50 mm, 3.5 μm) with an isocratic elution at a flow rate of 0.40 mL/min. The target analyte was completely separated by elution with 30 % acetonitrile containing 0.01 % NH 3 ·H 2 O and 1 mM NH 4 Ac for 3 min, without any endogenous interference. The method showed good linearity over the 0.020–50.0 μg/mL concentration range with a correlation coefficient r 2 = 0.9998. The intra-assay and inter-run precision and accuracy, recovery, and stability of the method were all within the acceptable parameters. Collectively, this study developed and validated a simple, fast, and sensitive LC-ESI-MS/MS method that did not require complex derivatization, acidification, large-volume sample consumption. Moreover, this method was successfully applied for routine urinary oxalic acid detection in children with kidney disease, providing valuable information for clinicians.
研究领域:
临床医学
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分析化学
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肾脏病学
✓ 已验证
产品关联
DOI
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 8
·e4256
·
IF 1.688
Fugeng Zhang,Xiaoli Qiao,Hui Lu,Shaoqiang Zhang,Wuxun Du,Xuefeng Xiao
Yiqifumai Injection is a lyophilized powder preparation widely used to treat coronary heart disease. However, its in vivo bioactive components and pharmacokinetic behavior remain unknown. Therefore a sensitive and specific LC–MS/MS was developed and validated for the simultaneous quantification of eight saponins and four lignans in beagle dog plasma. The plasma samples were pretreated by protein precipitation with methanol–acetonitrile (1:1, v /v). Chromatographic separation of all the 12 analytes and estazolam (internal standard, IS) was successfully accomplished on an Ultimate® XB-C 8 column (100 × 2.1 mm, 3 μm) with a gradient elution system. The total running time was 8 min with a flow rate of 0.40 mL/min. Acquisition of mass spectrometric data was performed via positive electrospray ionization in multiple reaction monitoring mode. The assay was fully validated in terms of selectivity, linear range, lower limit of quantitation, precision, accuracy, matrix effect, recovery and stability. This validated method was successfully applied to the pharmacokinetics of 12 bioactive components after intravenous administration of Yiqifumai Injection to beagle dogs at a dose of 0.541 g/kg.
研究领域:
药理学
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分析化学
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兽医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
·
2022
·
IF 6.056
Yujiao Yang,Pingling Zhang,Zhe Huang,Zhengang Zhao
Sterculia nobilis Smith pericarp is a by-product of tropical and subtropical fruit Sterculia nobilis Smith, the functional activity and phytochemical composition of which have not been widely reported. In this work, LC-ESI-MS/MS-MRM technique was used for the qualitative and quantitative analysis of 16 phenolic compounds in the ethyl acetate fraction of Sterculia nobilis Smith pericarp extract (EAF). Luteolin-7-O-glucoside, epicatechin gallate and apigetrin were the principal phenolics in the EAF. The hypoglycemic activity of EAF was examined by α-glucosidase and α-amylase inhibition models. EAF inhibited both α-glucosidase and α-amylase activities reversibly and uncompetitively with half-inhibitory concentration (IC 50 ) values of 69.390 ± 1.410 μg/mL and 2.151 ± 0.044 mg/mL, respectively. Enzyme inhibition mechanism of EAF was studied by spectroscopic methods. The results showed that EAF altered the secondary structure and microenvironment of tyrosine and tryptophan residues of the enzymes. This research demonstrates that Sterculia nobilis Smith pericarp is a potential raw material for production of functional foods at low cost.
研究领域:
药理学
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食品科学
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生物化学
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植物科学
✓ 已验证
产品关联
DOI
高影响因子
Current Analytical Chemistry
·
2016
·Vol. 12
·期 2
·159-166
·
IF 1.238
Pingting Li,Zhibin Tan,Xiaoling Gao,Shuqiang Liu,Shuling Wang
Context: Homocysteine (Hcy) is an amino acid that occurs in the body as an intermediate in the metabolism of methionine and cysteine. Hcyinplasma is a disease risk factor associated with both atherosclerosis and depression. The relation between Hcy balance and complication of atherosclerosis and depression remains unclear. Determination of Hcy in plasma is important and necessary for the research on comorbidities of atherosclerosis and depression. Objective: To establish an LC/ESI-MS/MS method for measuring plasma Hcy levels in rats and to compare plasma Hcy levels in rats exposed to high-fat diet, unpredictable mild stress or its combination. Materials and Methods: Forty rats were randomized into control group, high-fat group (HFD), chronic unpredictable mild stress group (CMS) and CMS+HFD group (n=10 in each group). 8 weeks later, the rats were sacrificed and plasma was collected for determining Hcy by LC/ESI-MS/MS. All data were analyzed by using SPSS13.0 software. Results: Compared to the plasma Hcy levels of control group, neither HFD group nor CMS group had statistical significance. However, CMS+HFD group showed a significantly higher level of plasma Hcy than the other three groups. Conclusions: Only when exposed to both high fat diets and chronic unpredictable mild stress, rats showed a remarkably elevated Hcy level in their plasma, however, when exposed alone to either high fat diet or chronic unpredictable mild stress, rats had a normal Hcy level in their plasma. Our findings indicate that Hcy is increased in comorbidity of atherosclerosis and depression.
研究领域:
生物化学
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精神病学
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心血管研究
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代谢组学
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分析化学
✓ 已验证
DOI
高影响因子
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
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2022
·
IF 5.895
Tong He,Peng Lei Cui,Jing Liu,Cheng Feng,Jian Ping Wang
In this study, a type of magnetic photoaffinity-labeled activity-based protein profiling probe for sulfonamide drugs was first synthesized for the purpose of capturing the natural dihydropteroate synthase of Escherichia coli by using simple incubation and magnetic separation. After characterization of its identity with LC-ESI-MS/MS, this enzyme was used as a recognition reagent to develop a direct competitive pseudo-ELISA for the determination of the residues of 40 sulfonamides in pork. Because of the use of streptavidin-horseradish peroxidase and biotinylated horseradish peroxidase as a signal-amplified system, the limits of detection for the 40 drugs were in the range of 0.001–0.016 ng/mL. Compared to the steps in a conventional assay formation, the operation steps were the same, but the sensitivities increased 32–88-fold. Furthermore, the assay performances were better than the previously reported immunoassays performances for sulfonamides. Therefore, this method could be used as a practical tool for multiscreening the trace levels of sulfonamides residues in food samples.
研究领域:
分析化学
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食品科学
·
生物化学
·
药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2015
·Vol. 7
·期 5
·2155-2161
·
IF 1.821
Hai-Long Li,Zhen-Miao Qin,Hong-Die Cai,Yin-Feng Tan,Xiao-Po Zhang,Yu-Chao Luo,Bei Li,Feng Chen,Jun-Qing Zhang
The evaluation of efficacy and safety should be paralleled with the assessment of comprehensive pharmacokinetic (PK) properties for a drug candidate, and a robust bioanalytical method is a prerequisite for obtaining PK information. α-Hederin is reported to have various in vitro and in vivo activities; however, very little is known about its PK and metabolic characteristics. In this study, we have developed an efficient LC-ESI(−)-MS/MS assay for α-hederin and its sapogenin hederagenin in rat plasma. Sample cleanup involved methanol precipitation for identification analysis and liquid–liquid extraction with ethyl acetate for quantification assay. LC analysis was performed under reversed-phase conditions in the modified “pulse gradient elution” mode. Analyte identification and quantification were conducted using multiple reaction monitoring (MRM) mode with euscaphic acid as the internal standard. Under these conditions, deglycosylated metabolites and their sulfate conjugates were detected; however, hederagenin was not detected in rat plasma samples after both oral and intravenous treatments. The mean plasma clearance (CL), volume of distribution (VSS) and elimination half-life (t1/2) of α-hederin were 0.24 L h−1 kg−1, 0.25 L kg−1 and 2.67 h, respectively. The oral bioavailability (F) of α-hederin in rats was about 0.14%, which might result from the poor intestinal absorption and/or extensive biliary excretion. It is hoped that this validated method will be useful for future PK studies of α-hederin.
研究领域:
药物分析
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药理学
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代谢组学
✓ 已验证
产品关联
DOI
高影响因子
Food Bioscience
·
2025
·
IF 5.9
Gaiwen Yu,Caimeng Zhang,Xingfei Li,Xiangzhen Kong,Yeming Chen,Yufei Hua
While soy yogurts offer health benefits, their wide market acceptance is limited by the less desirable flavor. This study investigated the generation of yogurt flavor volatiles and the metabolic pathways in the soymilk lactic acid bacteria (LAB) fermentation system, using dairy milk as a reference, through comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC × GC-TOFMS) and liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS)-based flavoromics and metabolomics. The results revealed that soy yogurts exhibited higher total volatile concentrations, but dairy yogurts demonstrated higher odor activity values (OAVs). Ten key metabolic pathways in soy-based fermentation, but 9 pathways in dairy-based system were identified. The pyruvate metabolism module served as a key node for the generation of yogurt flavor compounds in both systems; amino acid metabolic pathways were more active in soy than in dairy, while different carbohydrate metabolic pathways existed in soy-based and dairy-based systems. Expression levels of key enzymes for yogurt flavor formation were affected synergistically, antagonistically, or independently by the soy and dairy milk components. This work provides experimental evidence to solidify the theoretical framework of soymilk LAB fermentation.
✓ 已验证
产品关联
DOI
高影响因子
Analytical Methods
·
2014
·Vol. 6
·期 21
·8713-8721
·
IF 1.938
Feng Chen,Hai-Long Li,Yin-Feng Tan,Wei-Yong Lai,Zhen-Miao Qin,Hong-Die Cai,Yong-Hui Li,Jun-Qing Zhang,Xiao-Po Zhang
Euscaphic acid, a triterpene acid, exists ubiquitously in medicinal plants and demonstrates various pharmacological activities. This active compound is often used as a marker compound for quality control. Hitherto, the pharmacokinetic (PK) information is relatively scarce; therefore, it remains open to question whether the euscaphic acid reaches the target sites in the body at concentrations high enough for the claimed biological effects. A robust analytical method is prerequisite for obtaining enough PK information of euscaphic acid, which is useful for interpreting its pharmacological effects. In this study, we developed and validated a rapid liquid chromatographic tandem mass spectrometric (LC-MS/MS) method for the measurement of euscaphic acid in rat plasma. The rat plasma samples were precipitated with acetonitrile and the resulting supernatants were separated by a 4 min pulse gradient method on a Synergi Fusion-RP C18 column (4 μm, 2.0 mm i.d. × 50 mm). Ursolic acid was used as an internal standard for quantification of euscaphic acid. Deprotonated euscaphic acid and its internal standard were generated in negative electrospray ionization (ESI) mode and their precursor-to-product ion pairs (m/z 487.4→469.3 and 455.5→455.4, respectively) were used for measurement. Notably, the commonly used concentration of formic acid (HCOOH; 1‰ and 5‰, v/v) in the mobile phase seriously suppressed the signal intensity, but this mobile phase additive at a much lower concentration level (0.1‰ and 0.2‰) could overcome the matrix effects and therefore increase the sensitivity of MS detection of euscaphic acid. The newly developed bioanalytical assay possessed favorable accuracy and precision with a lower limit of quantification of 2.0 ng mL−1 and was successfully applied to PK studies in rats. The experimental strategies presented herein may be helpful for measurement of other triterpene acids in biological matrices.
研究领域:
分析化学
·
药理学
·
生物医学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2017
·
IF 3.255
Bing Chen,Xuewen Wang,Yulian Zou,Weiying Chen,Gang Wang,Wensong Yao,Peiying Shi,Shaoguang Li,Shilan Lin,Xinhua Lin,Hong Yao
Selaginella doederleinii Hieron is a widely used as folk Chinese medicine for treatment of different cancers. Our previous investigations have confirmed that the total biflavonoids in ethyl acetate extract from S. doederleinii (SDEA) have favorable anticancer potentials. However, the in vivo process of its bioactive ingredients remains unknown. In this paper, a sensitive and reliable method was developed for simultaneous quantification of main five biflavonoids, including amentoflavone , robustaflavone, 2″,3″-dihydro-3′,3″-biapigenin, 3′,3″-binaringenin and delicaflavone in the ethyl acetate extract of S. doederleinii (SDEA extract) in rat plasma by high-performance liquid chromatography with electrospray ionization-mass spectrometry (HPLC-ESI–MS/MS). Chromatographic separation was performed using an Ultimate ® XB-C18 (100 × 2.1 mm, 3.5 μm) with gradient elution of water (0.5% acetic acid) and acetonitrile at 0.2 mL/min. All analytes with internal standard (chrysin) were detected using selective reaction monitoring (SRM) in negative ionization mode. The method showed a good linearity over a wide concentration range (r 2 > 0.99). The limits of quantification for the biflavonoids were less than 10 ng/mL. The developed method was applied to the comparatively pharmacokinetic study of the five biflavonoids after oral or intravenous administration of SDEA extract in rats. In addition, in silico assessments of permeability and solubility of these biflavonoids were also performed to understand their poor bioavailability. It is the first time to report the in vivo process profiles of the biflavonoids of SDEA extract in rats.
研究领域:
药理学
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分析化学
·
中药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
DRUG DEVELOPMENT AND INDUSTRIAL PHARMACY
·
2021
·
IF 3.232
Xin Li,Huan Tong,Bing Xu,Yang Deng,Yuan Li,Junchen Huang,Yong Mao,Mengqin Liu,Ping Zhang,Siwei Guo
Budesonide is one of the intranasal corticosteroids, referred as first-line therapy for allergic rhinitis. Its determination is a challenging task due to its extremely low plasma levels, which limits the progress in the investigation of pharmacokinetics and quality control of preparations. In this study, a sensitive and high-throughput method to determine budesonide in human plasma using budesonide-d8 as the internal standard was developed and validated. A small volume of plasma sample (0.2 mL) was diluted with 0.2 mL water, followed by a solid-phase extraction using Cleanert PEP-2 products. Extracted samples were analyzed by liquid chromatography coupled to electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). Chromatographic separation of analytes was performed on an InertSustain AQ-C18 HP column (3 µm, 2.1 × 50 mm) under the reversed-phase condition with gradient elution. With the assay, linear calibration curves were obtained over the concentration range of 10–1200 pg/mL for budesonide, with considerable extraction recoveries (84.7–89.4%), and negligible matrix effects (<4.1). Moreover, the newly developed method was successfully applied to the evaluation of pharmacokinetics of two budesonide intranasal formulations with and without charcoal block in healthy volunteers.
研究领域:
药理学
·
分析化学
·
临床医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
CHEMICO-BIOLOGICAL INTERACTIONS
·
2019
·
IF 3.407
Wen-Jing Wu,Wei-Feng Tang,Ming-Hui Xiang,Jianshe Yan,Xiumei Cao,Chang-Hui Zhou,Yan Chang,Jing Xi,Yi-Yi Cao,Yang Luan,Xin-Yu Zhang
1-Chloro-2-hydroxy-3-butene (CHB) is a possible metabolite of 1,3-butadiene, a carcinogenic air pollutant . To demonstrate its formation in vivo, it is desirable to develop a practical biomarker and the corresponding analysis method. CHB can undergo alcohol dehydrogenase- and cytochromes P450 enzymes (P450)-mediated oxidation to yield 1-chloro-3-buten-2-one (CBO), which readily forms glutathione conjugates. We hypothesized that CBO-derived mercapturic acids , which are the expected biotransformed products of CBO-glutathione conjugates, could be used as CHB biomarkers. Thus, in the present study, we investigated the in vivo biotransformation of CHB into CBO-derived mercapturic acids. Because the reaction of CBO with N -acetyl- l -cysteine yields two products, 1,4- bis ( N -acetyl- S -cysteinyl)-2-butanone (NC1) and 1-chloro-4-( N -acetyl- S -cysteinyl)-2-butanone (NC2), we first developed an isotope dilution LC/ESI − -MS-MS method to quantitate urinary NC1 and NC2, and then determined their concentrations in urine of C57BL/6 mice and Sprague-Dawley rats administered CHB. Since no NC2 was detected in samples, the LC/ESI − -MS-MS method was optimized specifically for NC1. NC1 was enriched through solid phase extraction with the recovery being 75–82%. The limits of detection and quantitation were 6.8 and 34 fmol/0.1 mL for mouse urine, and 4.5 and 7.1 fmol/0.1 mL for rat urine, respectively. In urine of animals before CHB administration, no NC1 was detected; in mice administered CHB at 10 and 30 mg/kg, and rats at 5 and 15 mg/kg, NC1 was detected and its concentrations in urine from animals given higher doses were 3–6 fold higher than those given lower doses. Moreover, the NC1 concentrations in urine during 0–8 h were 4–6 fold and 10–11 fold higher than those during 8–24 h for mice and rats, respectively. The results demonstrated that CHB could be in vivo biotransformed into NC1, which could be used as a practical CHB biomarker.
研究领域:
毒理学
·
分析化学
·
环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）