Analytical Methods
·
2013
·Vol. 5
·期 22
·6395-6400
·
IF 1.855
Yilin Pan,Ping Xue,Xiang Li,Jianwei Chen,Jin Li
To establish an ultra-high performance liquid chromatography coupled with triple quadrupole mass (HILIC-UPLC-MS/MS) for determination of sixteen nucleosides and nucleobases in Isatidis Radix. Chromatographic separation was carried out on a Acquity UPLC BEH Amide column with gradient elution of acetonitrile (containing 0.1% acetic acid) and water (containing 0.8% acetic acid and 10 mmol L−1 ammonium acetate) at a flow rate of 0.3 mL min−1, the column temperature was set at 35 °C; Waters Xevo™ TQ worked in multiple reaction monitoring mode. Each component were separating in 11 min. All calibration curves were linear (r2 > 0.997) over the tested ranges. The limits of detection of these compounds were 0.02–42.54 ng mL−1. The limits of quantitation of these compounds were 0.05–98.18 ng mL−1. The average recoveries were in the range of 93.81–105.77% with RSD value less than 7.5%. The result showed that almost all of these Isatidis Radix were rich in nucleosides and nucleobases, but their contents were obviously various. The method was simple and fast with high precision, sensitivity and repeatability, which can be used for determination of this type class of nucleosides and nucleobases in other medicinal herbs.
研究领域:
药学
·
分析化学
✓ 已验证
DOI
高影响因子
Heliyon
·
2023
·
IF 4
Chengcheng Jin,Ting Wang,Tingting Zhao,Wen Jiang,Xiaolan Zhen,Hui Li
Objective To determine the concentrations of nine drugs used in the treatment of cardiovascular diseases in human plasma through QuEChERS pre-treatment combined with ultra-performance liquid chromatography-tandem mass spectrometry. Plasma samples were extracted with 3 mL of acetonitrile, 400 mg of anhydrous magnesium sulfate as a salting agent, and 20 mg of C18 as a sorbent. An Agilent Poroshell 120 EC-C18 column (4.6 × 100 mm, 2.7 μm) was selected and methanol-0.1 % water was used as the mobile phase, and ESI positive ion detection mode was selected. Results: The plasma concentrations of nisoldipine, metoprolol, and prazosin exhibited good linearity within the range of 0.05–4.0 ng/mL (r > 0.99), while atenolol, bisoprolol, propranolol, rosuvastatin, and atorvastatin showed linearity within the range of 0.5–40 ng/mL (r > 0.99). Fluvastatin showed good linearity within the range of 5.0–400 ng/mL. The accuracy of the method ranged from 94.15 to 110.62 %, while the recovery levels were in the range of 85.23 %–115.13 %. The matrix effects were observed between-6.54 % and 12.43 %. The intra-day and inter-day RSD was <15 % for the three concentrations of low, medium, and high. Conclusion The proposed method is rapid, accurate, specific, simple, reproducible, and suitable for the simultaneous measurement of the concentrations of nine drugs used in the treatment of cardiovascular diseases in human plasma.
研究领域:
分析化学
·
药理学
·
临床医学
✓ 已验证
DOI
高影响因子
Translational and Clinical Pharmacology
·
2021
·
IF 0
Hyeon-Cheol Jeong,Yo-Han Seo,Namyi Gu,Moo Yong Rhee,Kwang-Hee Shin
Candesartan and olmesartan are angiotensin II receptor blockers (ARBs) used for the treatment of hypertension and heart failure. Quantitation methods for candesartan and olmesartan were developed using ultra-high performance liquid chromatography-tandem mass spectrometry following protein precipitation. Candesartan was separated using 5 mM ammonium formate (A) and 100% acetonitrile (B) and olmesartan was separated using 2 mM ammonium formate with 0.1% formic acid (A) and 100% acetonitrile (B). Separation was performed using an isocratic method with a Thermo hypersil GOLD C18 column. Electrospray ionization was used for analyte ionization and detection of candesartan, olmesartan, and the internal standards by multiple reaction monitoring. Developed method showed excellent linearity ( r > 0.99) in the concentration range of 2–500 ng/mL for candesartan and 5–2,500 ng/mL for olmesartan. Accuracies were 86.70–108.8% for candesartan and 87.87–112.6% for olmesartan. These methods were able to successfully measure plasma candesartan or olmesartan concentrations in hypertensive patients. This study can be used for pharmacokinetic studies of candesartan or olmesartan in humans.
研究领域:
药理学
·
分析化学
✓ 已验证
DOI
PubMed
Foods
·
2025
·Vol. 14
·期 10
·1660
·
IF 5.1
Rong Chen,Lan Chen,Mingyue Du,Qiaozhen Guo,Ciping Zhong,Jing Zhang,Xiaoqin Yu
A high-throughput method for the determination of a variety of chemical hazards in poultry muscle and egg samples was established via ultra-performance liquid chromatography–tandem triple quadrupole mass spectrometry (UPLC–QqQ-MS). The sample preparation procedure was developed based on this quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and validated for 280 chemical hazards potentially present in poultry products. The target compounds in poultry samples were extracted with a 1% formic acid–acetonitrile solution (15:85,v/v), and the metal ions in the matrix were chelated by adding ethylenediaminetetraacetic acid disodium salt (Na2EDTA). The supernatant was purified using Enhanced Matrix Removal (EMR) lipid sorbent. Chromatographic gradient separation was performed on an ACQUITY UPLC BEH C18 (2.1 mm × 100 mm, 1.7 μm) column with multiple reaction monitoring (MRM) under both negative- and positive-ion mode. Internal standard calibration or matrix-matched calibration was used for the quantitation. The results showed that good linearity was achieved for each target compound with correlation coefficients (R2) ≥ 0.99. The limits of detection (LODs) ranged from 0.05 to 10 µg/kg, and the acceptable limits of quantification (LOQs) were determined to be 0.1–20 µg/kg for all 280 compounds. Approximately 90% of the target compounds exhibited mean recoveries ranging from 60% to 120%, with relative standard deviations (RSDs) within 16.2%. This method can be used for the high-throughput rapid detection of prohibited drug residues in poultry eggs due to its easy operation and high accuracy. It was applied in real sample detection, and 43 chemicals including metronidazole were found in 211 poultry samples, with a concentration range of 0.11–638 μg/kg.
研究领域:
食品科学
·
分析化学
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2021
·
IF 3.935
Qinghua Weng,Wei Tan,Ren-yue Yu,Ren-ai Xu,Yu Chen
Pemigatinib is an oral, selective, potent, competitive inhibitor acting on fibroblast growth factor receptor (FGFR)1, FGFR2, and FGFR3, which has obtained accelerated approval in the USA through a test approved by the USA FDA. It is not only significant in the therapy of adult recurrent, unresectable, metastatic or locally advanced cholangiocarcinoma, but also plays an important role in treating adult patients with FGFR2 fusion or other rearrangements. The aim of our research was to establish and verify a reliable and quick ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) assay to determine the level of pemigatinib in rat plasma. The analyte was prepared using a simple and convenient approach with acetonitrile for protein crash, and then separated from the matrix on a Waters Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) in a gradient elution program, where the mobile phase was consisted of acetonitrile and 0.1 % formic acid in water and was set at 0.40 mL/min flow rate. Selective reaction monitoring (SRM) was used to conducted for UPLC-MS/MS dectection with ion transitions at m / z 488.01 → 400.98 for pemigatinib and m / z 447.00 → 361.94 for erdafitinib (Internal standard, IS), respectively. This method had good linearity in a 0.5−1000 ng/mL calibration range for pemigatinib, where the lower limit of quantification (LLOQ) was validated at 0.5 ng/mL. The precision of pemigatinib for intra- and inter-day was less than 13.3 %, and the accuracy was determined to be from −4.8%–11.2%. During the assay in plasma samples, the analyte was found to be stable. Besides, matrix effect and recovery of the analyte and IS were acceptable. The novel optimized UPLC-MS/MS assay was also suitable for determining the concentration level of pemigatinib in a pharmacokinetic study after a single dose of 1.35 mg/kg pemigatinib orally to the rats.
研究领域:
药物分析
·
生物化学
·
医学研究
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2014
·
IF 2.694
Wei-min Zhang,Rui-fang Li,Ming Sun,Da-ming Hu,Jian-fei Qiu,Yun-hao Yan
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 avicularin in rat plasma. Sample preparation was accomplished through a simple one-step deproteinization procedure with 0.2 mL of acetonitrile–methanol (9:1, v/v) 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 1.60 min and the elution of avicularin was at 1.20 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 434.1 → 301.3 for avicularin and m / z 237.2 → 194.3 for carbamazepine (IS), respectively. The calibration curve was linear over the range of 10–3000 ng/mL with a lower limit of quantitation (LLOQ) of 10 ng/mL. Mean recovery of avicularin in plasma was in the range of 84.2–89.5%. Intra-day and inter-day precision were both <12%. This method was successfully applied in pharmacokinetic study after intravenous administration of 5.0 mg/kg avicularin in rats.
研究领域:
分析化学
·
药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
CyTA-Journal of Food
·
2025
·
IF 1.7
Zhou Lu,Zhao Junpeng,Hilary Kwesi Ketemepi
A QuEChERS-UPLC-MS/MS method was developed and validated for simultaneous determination of six pesticides (chlorpyrifos, malathion, carbofuran, thiodicarb, deltamethrin, and lambda-cyhalothrin) in dairy products. Samples (n=50), collected from a supermarket in Chongqing, China, were extracted with 1% acetic acid–acetonitrile, purified using PSA, and quantified by external-standard UPLC-MS/MS. All pesticides showed excellent linearity (0.001–0.50 mg/L, R² > 0.99), with LOQs of 0.002 mg/kg. Average recoveries at four spiking levels (0.002, 0.01, 0.1, 1.0 mg/kg) ranged from 89% to 110% (RSD 0.5–9.5%, n=5). Analysis of real samples revealed residues below China’s MRLs (GB 2763–2021), confirming regulatory compliance. The method meets analytical requirements for dairy matrices and offers a reliable framework adaptable to other international standards.
研究领域:
食品科学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
Journal of Chemistry
·
2019
·
IF 1.727
Hongbin Guo,Mengqiao Chen,Mengran Li,Mingye Hu,Baohua Chen,Chengyan Zhou
Mangiferin (MG) is an active component in natural medicines, and various studies have been reported on pharmacological effects, but the low solubility and bioavailability of MG limit its wide application. The aim of the present study was to investigate the pharmacokinetic profiles of mangiferin (MG) and mangiferin monosodium salt (MG-Na) in rat plasma by UPLC-MS/MS, which were then compared between the two groups. An appropriate high sensitivity and selectivity ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was applied to the comparison of plasma pharmacokinetics in MG and MG-Na using carbamazepine as internal standard (IS). These results showed that there were statistically significant differences in the pharmacokinetic parameters between MG and MG-Na after a single oral administration at 100 mg/kg. When compared with pharmacokinetic parameters of MG, the AUC(0-t), AUC(0–∞), Cmax,K10, and Ka of MG-Na were increased by 5.6-, 5.7-, 20.8-, 8-, and 83.6-fold, while the Tmax and CL/F were decreased by 4- and 5.7-fold (), respectively. t1/2 value showed an increasing trend, but was statistically significant between the two groups. Moreover, the AUC value in the MG-Na group was significantly increased and the relative bioavailability was calculated to be 570% when compared with that of the MG group. These results suggested that the salification reaction of MG can effectively enhance gastrointestinal absorption and relative bioavailability by improving solubility and membrane permeability.
研究领域:
药理学
·
分析化学
✓ 已验证
DOI
高影响因子
Natural Product Communications
·
2024
·
IF 1.5
Meng S. Cheong,Lutfun Nahar,Satyajit D. Sarker,Hui Cao,Wai S. Cheang,Jianbo Xiao
Piceatannol is a stilbenoid, which has shown bioactivities in various cell culture models. However, its stability in cell culture medium is not clear. Here, UPLC-MS/MS was applied in situ to analyze the degradation products of piceatannol in Dulbecco's Modified Eagle's Medium (DMEM) and cell culture to investigate the compound's stability in DMEM. During the incubation with cell culture medium (at 4 and 37 °C), several piceatannol derivatives, such as an oxidation product (m/z 243.06), a reduction product (m/z 247.09), dimers (m/z 485.12 and 487.14) and trimers (m/z 727.18) were detected, which demonstrated the instability of piceatannol in cell culture conditions. To confirm if the new products during the incubation were generated due to the instability of piceatannol, ascorbic acid was added. The presence of ascorbic acid could significantly slow the degradation rate of piceatannol and the generation of piceatannol derivatives, which proved that the new products were generated by the degradation of piceatannol and indicated that the instability of piceatannol might be related to its antioxidant activity.
研究领域:
生物化学
·
药物化学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2021
·
IF 4.821
Yueting Liao,Yaohai Zhang,Qiyang Zhao,Wei Xiang,Bining Jiao,Xuesu Su
Metal organic framework MIL-101(Cr) was successfully synthesized as a selective adsorbent by a facile self-assembly technique and combined with UPLC-MS/MS for enrichment and determination of neonicotinoids in fruit juices and tea beverages. Therein, MIL-101(Cr) was characterized by Fourier transform infrared spectrometry, scanning electron microscopy, X-ray diffraction, and N 2 adsorption–desorption isotherms. Box-Behnken design was applied to optimize the significant variables including the sorbent amount, pH of the matrix, eluant volume, extraction time and desorption time. The optimized conditions were sorbent amount of 20 mg, eluent volume of 1 mL, extraction time of 5 min and desorption time of 4 min. Under the optimized conditions, excellent sensitivity was achieved with the limit of detection of 0.0019–0.02 μg/L and limit of quantification of 0.0063–0.067 μg/L. Good linearity (R 2 ≥ 0.9988) was obtained within the range of 1–1000 μg/L, and the recovery was 71.04%-101.64% with relative standard deviations (RSDs) of 1.25%-8.82% in spiked samples. The inter- and intra-day RSDs were both<8.54%. The adsorption isotherms investigated for acetamiprid, thiacloprid, and imidacloprid pesticides better fitted with the Freundich adsorption isotherm with bimolecular adsorption capacity of 71.43, 68.49, and 50.38 mg/g, respectively. These results indicate that the nanocomposite is feasible for adsorption of the target analytes at trace amounts from fruit juices and tea beverages.
研究领域:
分析化学
·
环境科学
·
食品科学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2024
·
IF 4
Yifu Jiang,Le Lang,Jingwen Zhang,Yining Ji,Chenglong Zhang,Ruiqin Yang,Xuwen Li
This study combined the structural characteristics of amanita peptide toxins to prepare a Fe 3 O 4 /P4VPBA/PPy/GO composite material as a magnetic solid-phase extraction adsorbent. The experimental results indicated that this adsorbent showed excellent selectivity for the extraction of amatoxins and phallotoxins from mushroom samples. Compared with traditional dispersive solid-phase extraction, this adsorbent enables rapid separation in the enrichment and elution recovery stages through the application of a magnetic field . Simultaneously, the study optimized the conditions for ultraperformance liquid chromatography–mass spectrometry (UPLC–MS/MS), ensuring both separation efficiency and accuracy while reducing the analysis time. The researchers established the MSPE–UPLC–MS/MS method for the determination of amanita peptide toxins in wild mushrooms. This method not only simplified and expedited the sample pretreatment process but also achieved qualitative and quantitative analyses in a short period, thus demonstrating high detection sensitivity and outstanding recovery rates. Furthermore, the developed method was successfully applied to analyze toxic mushrooms discovered in Nanjing, China. The potential for extensive utilization of this method is highlighted in the field of food analysis and detection.
研究领域:
分析化学
·
食品科学
·
毒理学
✓ 已验证
产品关联
DOI
高影响因子
Food Chemistry-X
·
2022
·
IF 6.443
Tao Zheng,Jia-qian Sun,Xiao-jun Shi,Du-ling Liu,Bing-yin Sun,Yuanjie Deng,Ding-ling Zhang,Shu-ming Liu
Through field investigation, UPLC-MS/MS technology and MaxEnt model were performed to predict the suitable distribution area for red huajiao ( Zanthoxylum bungeanum maxim.) in China from 2021 s to 2060 s, and evaluate the effects of climate factors on the quality of red huajiao. The results demonstrated that mean temperature of the coldest quarter and min temperature of the coldest month were the most important environmental variables influencing red huajiao distribution. Suitable habitats for red huajiao were located mainly in dry and hot valley zone in the Qinba Mountains and the semi-humid and semi-arid areas of the Loess Plateau. The amides contents were higher in high suitability areas, while it was decreased in medium and low suitability areas, and temperature, wind speed and precipitation played a key role in their accumulation. This investigation was of great significance for the planting area optimization, quality control, benefit improvement and industrial development of red huajiao.
研究领域:
植物学
·
生态学
·
药用植物研究
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）