JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2019
·Vol. 58
·期 1
·31-36
·
IF 1.216
Zhou Li,Xi Wang,Zhang Hui,Sun Lili,Yu Jinlong,Zou Qiaogen
A simple and enantioselective method was developed and validated for the simultaneous determination of (R)- and (S)-trelagliptin in beagle dog plasma by chiral liquid chromatography tandem mass spectrometry. Trelagliptin enantiomers and (R)-rabeprazole (as internal standard, IS) were extracted from plasma samples by liquid–liquid extraction and separated on a CHIRALCEL OX-3R column using acetonitrile-5 ammonium bicarbonate as the mobile phase in gradient elution mode. The multiple reactions monitoring transitions of m/z 358.1→341.2 and 359.9→150.1 were used to quantify trelagliptin enantiomers and IS, respectively. This method was validated for sensitivity, specificity, linearity, precision, accuracy and stability of specific analytes under various conditions. And it was successfully applied to evaluating the pharmacokinetic profile of trelagliptin enantiomers in beagle dogs after single intravenous administration of (R)-trelagliptin injection (at 1 mg/kg) and oral administration (at 6.7 mg/kg). In this study, no chiral bioconversion of (R)-trelagliptin to (S)-trelagliptin in beagle dog plasma was observed. The absolute bioavailability of (R)-trelagliptin was identified to be 128.2%.
研究领域:
药物分析
·
药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF ANALYTICAL TOXICOLOGY
·
2015
·Vol. 39
·期 7
·551-556
·
IF 2.858
Wang Ting,Yu Zhiguo,Shi Yan,Xiang Ping
At the global level, seizures of crystalline methamphetamine (MA) and MA tablets have risen to a new high, indicating that the substance is an imminent threat. MA enantiomer profiling was a useful tool to investigate the prevalence of MA abuse, the intrinsic characteristics of the seized samples and the trends of precursors. In this work, the distribution of enantiomers in clandestine MA crystals and tablets seized mainly in the Yangtze River Delta region, China, from 2008 to 2014 were identified. The MA samples were diluted with internal standard methanol solution, and analyzed by LC–MS-MS. The detection limits of the enantiomers were 0.04 μg/L. The limit of quantification was 0.1 μg/L. As little as 0.2% of the R-enantiomer ratio could be determined. Standard calibration curves of S- and R-MA showed good linearity in the range of 0.1–80 μg/L (r2 > 0.995). All of the seizures were optically pure S-enantiomer in the years 2008 and 2009. Seized samples containing a slight amount of R-MA began to appear in 2010 and increased in the year 2014. No racemic mixture or R-isomer of MA was seized. From this study, we could find out that smuggling routes and/or precursors might be silently changing in the Yangtze River Delta region, China.
研究领域:
分析化学
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法医学
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药学
✓ 已验证
产品关联
DOI
PubMed
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
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2023
·Vol. 37
·期 4
·e5584
·
IF 1.8
Kaiyue Ren,Yanjuan Yuan,Qing Shao,Hongqun Qiao
For the further study of [ 19 F] - alfatide, the development of highly sensitive analytical methods for its determination is an urgent issue. In this paper, a method for simultaneously determining [ 19 F]-alfatide and alfatide using liquid chromatography/tandem mass spectrometry was created and validated. The plasma samples were pretreated using the protein precipitation method. Poroshell 120 EC-C 18 (4.6 × 50 mm, 2.7 μm, Agilent) was used for the separation of the analytes to be measured. The mobile phase, consisting of acetonitrile and water (0.1% acetic acid, 50:50, v/v), was delivered at a flow rate of 0.60 ml/min for sample analysis. Positive electrospray ionization was performed using multiple-reaction monitoring with transitions of m / z 715.2 → 636.6 for [ 19 F]-alfatide, the ion pairs 700.3 → 851.5 for alfatide and the ion pairs 237.1 → 194.2 for carbamazepine (internal standard). According to the results, the method had high specificity, precision and accuracy as well as an extended linear range. The matrix effect and extraction recovery were also acceptable. The method was successfully applied to the pharmacokinetic study of [ 19 F]-alfatide in rats.
研究领域:
分析化学
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药理学
·
药物代谢
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF LIPID RESEARCH
·
2022
·Vol. 63
·期 12
·
IF 6.676
Xian Fu,Hou-Hua Yin,Ming-Jun Wu,Xin He,Qing Jiang,Ling-Tong Zhang,Jun-Yan Liu
Oxylipins are important biological regulators that have received extensive research attention. Due to the extremely low concentrations, large concentration variations, and high structural similarity of many oxylipins, the quantitative analysis of oxylipins in biological samples is always a great challenge. Here, we developed a liquid chromatography-tandem mass spectrometry-based method with high sensitivity, wide linearity, and acceptable resolution for quantitative profiling of oxylipins in multiple biological samples. A total of 104 oxylipins, some with a high risk of detection crosstalk, were well separated on a 150 mm column over 20 min. The method showed high sensitivity with lower limits of quantitation for 87 oxylipins, reaching 0.05–0.5 pg. Unexpectedly, we found that the linear range for 16, 18, and 17 oxylipins reached 10,000, 20,000, and 40,000 folds, respectively. Due to the high sensitivity, while reducing sample consumption to below half the volume of previous methods, 74, 78, and 59 low-abundance oxylipins, among which some were difficult to detect like lipoxins and resolvins, were well quantified in the tested mouse plasma, mouse liver, and human plasma samples, respectively. Additionally, we determined that analytes with multifarious concentrations of over a 1,000-fold difference could be well quantified simultaneously due to the wide linearity. In conclusion, most likely due to the instrumental advancement, this method effectively improves the quantitative sensitivity and linear range over existing methods, which will facilitate and advance the study of the physiological and pathophysiological functions of oxylipins.
研究领域:
分析化学
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生物化学
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药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Antioxidants
·
2019
·Vol. 8
·期 8
·321
·
IF 4.52
Dandan Wang,Liangxiao Zhang,Yueqing Xu,Xin Qi,Xuefang Wang,Xiupin Wang,Qi Zhang,Peiwu Li
Sesame is a nutritional agricultural product with medicinal properties. Accurate determination of micronutrients is important for the improvement of sesame quality and nutrition assessments. Our previous study showed that 10 antioxidants—d-homoproline, vitamin B2, coniferyl aldehyde, hesperidin, phloretin, N-acetyl-l-leucine,l-hyoscyamine, ferulic acid, 5-methoxypsoralen, and 8-methoxypsoralen—in sesame were potential characteristic nutrients in sesame. Herein, simultaneous detection of 10 different types of antioxidants was developed by using ultrasound-assisted extraction coupled with liquid chromatography-tandem mass spectrometry (UAE-LC-MS/MS) with the help of response surface methodology. The significant variables and levels were screened and optimized by combining the single factor experiment, Plackett–Burman test, and Box–Behnken design. The optimal conditions for extraction of target antioxidants in sesame were methanol solution of 75.0%, liquid-to-material ratio of 20:1 (mL/g), extraction temperature of 50 °C, extraction power of 410.0 W, extraction time of 65 min. The total yield of targets was 21.74 μg/g under the optimized conditions. The mobile phase used was 0.1% formic acid in acetonitrile and 0.1% formic acid in water, and the column was a Thermo Syncronis C18 reverse phase column (100 mm × 2.1 mm, 3 μm). All targets required only one injection and could be quickly separated and assayed within 7 min. The limits of detection and limits of quantification for these 10 nutritional compounds ranged from 0.01 to 0.11 µg/kg and from 0.04 to 0.34 µg/kg, respectively. The validation results indicated that the method had reasonable linearity (R2≥ 0.9990), good recoveries (71.1%–118.3%), satisfactory intra-day precision (≤9.6%) and inter-day precision (≤12.9%), and negligible matrix effects (≤13.8%). This simultaneous quantification method was accurate, fast, and robust for the assessment of sesame nutrition.Keywords:antioxidants;ultrasound-assisted extraction;liquid chromatography-tandem mass spectrometry (LC-MS/MS);sesame;simultaneous detection;response surface methodology
研究领域:
食品科学
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分析化学
·
营养学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2018
·Vol. 185
·期 6
·1-10
·
IF 5.705
Yang Wen,Li Tengfei,Shu Chang,Ji Shunli,Wang Lei,Wang Yan,Li Duo,Mtalimanja Michael,Sun Luning,Ding Li
A method is described for the determination of proteins with LC-MS/MS enabled by a small molecule (adenosine) barcode and based on a double-recognition sandwich structure. The coagulation protein thrombin was chosen as the model analyte. Magnetic nanoparticles were functionalized with aptamer29 (MNP/apt29) and used to capture thrombin from the samples. MNP/apt29 forms a sandwich with functionalized gold nanoparticles modified with (a) aptamer15 acting as thrombin-recognizing element and (b) a large number of adenosine as mass barcodes. The sandwich formed (MNP/apt29-thrombin-apt15/AuNP/adenosine) can ben magnetically separated from the sample. Mass barcodes are subsequently released from the sandwiched structure for further analysis by adding 11-mercaptoundecanoic acid. Adenosine is then detected by LC-MS/MS as it reflects the level of thrombin with impressively amplified signal. Numerous adenosines introduced into the sandwich proportional to the target concentration further amplify the signal. Under optimized conditions, the response is linearly proportional to the thrombin concentration in the range of 0.02 nM to 10 nM, with a detection limit of 9 fM. The application of this method to the determination of thrombin in spiked plasma samples gave recoveries that ranged from 92.3% to 104.7%.
Schematic representation of a method for the determination of thrombin with LC-MS/MS. The method is based on a double-recognition sandwiched structure. With LC-MS/MS, mass barcodes (adenosine) are detected to quantify thrombin, which amplifies the detection signal impressively.
研究领域:
分析化学
·
蛋白质组学
·
医学检测
✓ 已验证
DOI
PubMed
高影响因子
Results in Chemistry
·
2026
·
IF 5.8
Xiaozheng Huang,Ruizi Qing,Yuqing Sun,Yuanqing Wei,Rui Liu,Shuying Han,Yuhao Teng
Accurate absolute quantification of peptides in complex matrices using LC-MS/MS is often hindered by significant matrix effects, especially in the quantitative determination of gelatin peptides in food. This study developed a strategy to reduce matrix interference in LC-MS/MS quantification of gelatin peptides by screening a simulated matrix based on physicochemical similarity. Deer antler gelatin was hydrolyzed with eight proteases and comprehensively characterized. Multivariate analyses (PCA and HCA) identified the Compound proteinase hydrolysate as most closely resembling the Trypsin-digested matrix with minimal interference, and was selected for method development. The validated method for five characteristic peptides showed excellent linearity (12.5–500 ng/mL, r 2 > 0.998), with LOQs of 0.12–5.20 ng/mL, precision RSDs of 4.45–12.44%, and accuracy of 79.5–116.9%. It was successfully applied to quantify peptides in Cervidae antler gelatin, thereby providing a practical approach to improving reliability in food quality control.
✓ 已验证
DOI
高影响因子
RSC Advances
·
2025
·Vol. 15
·期 21
·16973-16982
·
IF 4.6
Haijun Wang,Qiao Zhang,Xiaolin Li,Huan Chen,Xiaolan Zhu,Liming Yang,Hongling Yin,Jing Sun,Shuhong Fang,Hui Zhang
A large-volume direct-injection (LVDI) method was developed and validated for the simultaneous analysis of 69 antibiotics in bottled water using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Target antibiotics included 23 sulfonamides, 19 quinolones, 12 macrolides, 11 β-lactams, and 4 tetracyclines. Optimization of ion source parameters led to enhanced signal intensities for 55 antibiotics. The 100 μL injection volume was both feasible and preferred, resulting in increased signal intensities while maintaining unchanged peak shapes for the antibiotics. Good absolute recoveries for the 69 antibiotics were obtained with the LVDI method, primarily ranging from 80% to 120%, whereas lower absolute recoveries of macrolides, quinolones, sulfonamides and β-lactams were observed with a solid-phase extraction (SPE) method. The limits of detection (LODs) for antibiotics were generally comparable between the LVDI and SPE methods, with values below 1 ng L−1 for most antibiotics (0.00271–26.6 ng L−1). Analysis of 25 brands of bottled water using the LVDI method revealed the presence of 54 antibiotics from 5 classes, with detection frequencies (DFs) ranging from 4% to 100% and detected concentrations between 0.0453 and 37.4 ng L−1. Multiple antibiotics were detected simultaneously in bottled water, with more than 10 antibiotics identified in each of 9 different brands. Quinolones and sulfonamides were the predominant antibiotics, accounting for over 80% of the total concentration. Only sulfaclozine showed significantly different concentrations between purified drinking water and natural mineral water (22.2 vs. 17.2 ng L−1, p < 0.05).
研究领域:
分析化学
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环境科学
·
食品科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Yu Qin,Shenping Zhang,Jingwen Shi,Heng Gong
Antibiotics are a class of compounds that are effective against bacterial infections and are widely used in aquaculture. Herein, a method based on high performance liquid chromatography coupled with tandem mass spectrometry was developed to detect nine classes of 116 antibiotics in aquatic products. The antibiotics were extracted in two steps using 1% formic acid-acetonitrile with 0.1 mol/L Na 2 EDTA-Mcllvain buffer solution and acetonitrile, purified using Captiva EMR-Lipid, and separated with an ACQUITY UPLC®HSS T 3 column (100 mm×2.1 mm, 3.5 μm) using acetonitrile and 0.1% formic acid with 5 mM ammonium acetate as mobile phase for gradient elution. Calibration curve from 0.10 to 100 ng/mL exhibited good correlation coefficient (R 2 >0.99) for quantification. The analytical performance of the developed method was satisfactory, with limits of quantification ≤ 5.00 ng/g for detecting of antibiotics in aquatic products. The recoveries of the 116 antibiotics ranged from 60.57% to 127.33%, with precision (expressed as relative standard deviation) of < 30.20%. All parameters showed acceptable values and conformed to the Commission Decision 2021/808/EC criteria. When compared with other techniques, the developed method meets the quantitative requirements of high-throughput analysis and can simultaneously analyze 116 antibiotics in aquatic products.
研究领域:
分析化学
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食品科学
·
环境科学
·
药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Frontiers in Plant Science
·
2024
·
IF 4.1
Qian Huimin,Hu Yan,Zhang Haiwen,Chu Shanshan,Peng Huasheng
Gardeniae Fructus (Zhizi) serves as both a medicinal and edible substance and finds widespread use in various industries. There are often two kinds of medicinal materials in the market: Zhizi and Shuizhizi. Typically, Zhizi with small, round fruit is used for medicinal purposes, while Shuizhizi, characterized by large, elongated fruit, is employed for dyeing. Market surveys have revealed a diverse range of Zhizi types, and modern research indicates that Shuizhizi contains rich chemical components and pharmacological activities. In this study, we collected 25 batches of Zhizi and Shuizhizi samples, categorizing them based on appearance into obovate and round fruits, with seven length grades (A–G). Using the ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-QQQ-MS/MS) method, we simultaneously quantified 13 main chemical components in fruits of Gardenia species. In addition, we compared the weight percentage of the pericarp, flesh, and seeds parts of samples with different traits, and quantified 13 chemical components in different parts. Results indicated that, aside from a few instances of overlapping fruit size ranges, Shuizhizi generally exhibits larger and longer dimensions than Zhizi. The weight proportion of the Shuizhizi pericarp is often higher than that of the Zhizi pericarp. Quantitative results highlighted significant differences in the chemical component content between Zhizi and Shuizhizi, with Shuizhizi generally containing higher levels of iridoids. The PCA and OPLS-DA analysis distinctly divided Shuizhizi and Zhizi, among which three iridoids, two organic acids, and one flavonoid made significant contributions to their classification. Cluster heatmap analysis also demonstrated complete separation between Zhizi and Shuizhizi, with clear distinctions among Zhizi samples from different origins. The distribution of the 13 chemical components in different Zhizi and Shuizhizi parts remained consistent, with iridoids and pigments concentrated in the seeds and flesh, and two organic acids and one flavonoid enriched in the pericarp. In summary, this study contributes valuable insights for classifying Zhizi and offers guidance on the rational use of Shuizhizi and the different parts of Zhizi.
研究领域:
药理学
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分析化学
·
中药学
·
植物学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2024
·Vol. 29
·期 13
·3133
·
IF 4.2
Qimei Wu,Jinfen Zheng,Yan Yu,Zhirong Li,Ying Li,Chengfeng Hu,Yaping Zhou,Rongxiang Chen
Vitex negundohas strong antioxidant activity, but its primary antioxidant components are not clear. In this study, the antioxidant components were screened by offline two-dimensional liquid chromatography coupled with electrochemical detection (2D-LC-ECD) and subsequently assessed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) identification, radical scavenging capacity, and molecular docking. Various fractions were isolated fromVitex negundoleaves, and 39 antioxidant components were screened and identified. All of the fractions containing the antioxidant components exhibited certain antioxidant activity. Correlation analysis revealed a strong correlation between the response of LC-ECD and the in vitro antioxidant activity of the fractions. Molecular docking demonstrated that components with high response to LC-ECD exhibited robust interaction with antioxidant-related target proteins. The main antioxidant components ofVitex negundoleaves were isoorientin, chlorogenic acid, agnuside, cynaroside, and scutellarin. The 2D-LC-ECD combined with LC-MS/MS was rapid and effective in screening the antioxidant components inVitex negundoleaves and could also provide technical support for the discovery of antioxidant components with different polarities and contents in other medicinal and edible plants.
研究领域:
植物化学
·
分析化学
·
药理学
✓ 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）