RSC Advances
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2022
·Vol. 12
·期 15
·9256-9262
·
IF 4.036
Mengmeng Zhao,Xiaoxia Wu,Zengda Yu,Yunkai Sun,Zhao Liu,Jinqiao Yuan,Hu Liu,Yiping Jin
Avanafil is a phosphodiesterase type 5 inhibitor which is used to treat erectile dysfunction in men. The process-related impurities of avanafil were investigated, and four kinds of impurities in several laboratory batches with a content of 0.29–1.63% were detected by the newly developed gradient ultra-high performance liquid chromatography (UPLC). Based on the synthesis route and UPLC-MS research, the impurities are inferred as Imp-A, Imp-B, Imp-C and Imp-D. The structures of the impurities were inferred from LC-MS studies and confirmed by synthesis, followed by spectroscopic characterization such as NMR and mass spectrometry. Especially, the synthesis of Imp-D is firstly reported. The drug-related substances can be separated well by efficient and selective ultra-high performance liquid chromatography on a Waters ACQUITY HSS C18 (50 × 2.1 mm, particle size 1.8 μm) column at 35 °C, with the mobile phase consisting of ammonium formate (20 mM) and acetonitrile, and the detection at 239 nm with a DAD detector. The method was validated in terms of specificity, linearity, precision, accuracy and sensitivity, and satisfactory results were obtained. The results indicated this developed UPLC method for avanafil and the proposed synthesis mechanism can be used for quality control purposes as required by regulatory agencies to ensure the safety and efficacy of the product.
研究领域:
药物化学
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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
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2025
·
IF 2.8
Meichen Liu,Yingxia Guo,Ziyi Niu,Yufeng Guo,Shuang Feng,Xiaoyan Zhang,Jiansong You,Lei Yin,Hongyu Xue,Meiyun Shi
A sensitive and selective ultra-performance liquid chromatography-tandem mass spectrometry cubed (UPLC-MS 3 ) assay was established for detection of fipronil in zebrafish tissue samples. Following protein precipitation pretreatment, the concentrations of fipronil in various zebrafish tissue samples were quantified by the developed UPLC-MS 3 assay. Fipronil was monitored by MS 3 transition ( m/z 435.0 → 398.9 → 330.0) with a ± 1.0 Da isolation window for secondary product ions. Chromatographic separation was achieved with 0.1 % formic acid-water ( v /v) as the aqueous phase and acetonitrile as the organic phase. Gradient elution with C 18 column was employed for separation of fipronil and probenecid (internal standard, IS). Method validation demonstrated excellent linearity over the range of 0.1–10 ng/mL (r 2 > 0.995), with the accuracies ranging from −10.33 % to 3.17 % and precisions between 3.25 % and 11.34 %. Consistent extraction recoveries (89.92–113.49 %) and acceptable matrix effects (92.54–110.27 %) were observed across all tested matrices. The implementation of MS 3 scanning significantly enhanced specificity by eliminating endogenous interference compared to conventional MRM detection. The successful application of this method in zebrafish tissue distribution studies confirmed its reliability for environmental toxicology research. This MS 3 -based approach provides a robust analytical platform for investigating biodistribution of fipronil in aquatic models.
研究领域:
分析化学
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环境科学
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毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Separations
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2022
·Vol. 9
·期 6
·140
·
IF 3.344
Xue Li,Wei Wang,Suling Sun,Junhong Wang,Jiahong Zhu,Feng Liang,Yu Zhang,Guixian Hu
A method for quantifying the anthocyanins in grapes was firstly developed by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOFMS) combined with quantitative analysis of multi-components by single marker (QAMS). A total of 10 main anthocyanins were analyzed by using peonidin 3-O-glucoside as the reference standard. The accuracy of this method was evaluated by an established and validated external standard quantification method with 10 reference compounds. The standard method difference (SMDs) of the quantification results between QAMS and the external standard methodwasless than 15%. Furthermore, the QAMS method was used to analyzefour batches of grapes and the data was compared with those obtained using the external standard method. No significant difference wasobtained in the results obtained by both methods. These results indicated that the QAMS method could accurately determine the anthocyanins in grapes. This method can provide a basis to address the absence of reference standards for analyzing anthocyanins in other foods.
研究领域:
食品科学
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分析化学
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植物学
✓ 已验证
DOI
高影响因子
Analytical Methods
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2013
·Vol. 5
·期 22
·6395-6400
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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
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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
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药理学
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临床医学
✓ 已验证
DOI
高影响因子
MOLECULES
·
2019
·Vol. 24
·期 16
·3016
·
IF 3.06
Ying Xue,Lin-Sen Qing,Li Yong,Xian-Shun Xu,Bin Hu,Ming-Qing Tang,Jing Xie
So far, there is no report on the quality evaluation of lemonade available in the market. In this study, a sample preparation method was developed for the determination of flavonoid glycosides by ultra-performance liquid chromatography–mass spectrometry (UPLC-MS) based on vortex-assisted dispersive liquid-liquid microextraction. First, potential flavonoids in lemonade were scanned and identified by ultra-performance liquid chromatography–time of flight mass spectrometry (UPLC-TOF/MS). Five flavonoid glycosides were identified as eriocitrin, narirutin, hesperidin, rutin, and diosmin according to the molecular formula provided by TOF/MS and subsequent confirmation of the authentic standard. Then, an ultra-performance liquid chromatography–triple quadrupole mass spectrometry (UPLC-QqQ/MS) method was developed to determine these five flavonoid glycosides in lemonade. The results showed that the content of rutin in some lemonade was unreasonably high. We suspected that many illegal manufacturers achieved the goal of low-cost counterfeiting lemonade by adding rutin. This suggested that it was necessary for relevant departments of the state to make stricter regulations on the quality standards of lemonade beverages.Keywords:vortex-assisted dispersive liquid-liquid microextraction;flavonoid glycoside;UPLC-MS;counterfeiting lemonade
研究领域:
分析化学
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食品科学
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药物分析
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CONTROL
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2021
·
IF 5.548
Yaqi Hou,Jiao Liu,Yanchun Shao,Xitian Peng,Dawen Zhang,Lifang Hu,Fusheng Chen,Youxiang Zhou
Modified mycotoxins can cause an underestimation of exposure risk due to their untraceable characteristics. Hongqu , a traditional Chinese fermented product, is widely used as food colorants , fermenters and functional foods for about 2000 years. Though there were several methods to reduce citrinin (CIT) content in Hongqu , the risk assessment and prevention of modified CIT remain inadequate, causing potential risk to human health. The current study firstly identified the occurrence of modified CIT in Hongqu via acid, alkaline and enzyme hydrolysis combined with chromatographic and mass spectrometric approaches. Then 8 Hongqu samples and 5 Monascus products were treated using the optimized acid hydrolysis method and analyzed by ultra-high-performance liquid chromatography with fluorescence detector. The results showed that CIT content in the CIT positive Hongqu increased by 35.28%–458.13% after acid hydrolysis, demonstrating there could be a underestimation risk in the CIT positive Hongqu samples, and the modification of CIT might not be chemical modified, but matrix associated.
研究领域:
食品安全
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微生物学
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毒理学
✓ 已验证
产品关联
DOI
高影响因子
Translational and Clinical Pharmacology
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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
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分析化学
✓ 已验证
DOI
PubMed
MOLECULES
·
2020
·Vol. 25
·期 5
·1082
·
IF 3.267
Limin Li,Bin Hao,Yulong Zhang,Shen Ji,Guixin Chou
Militarine, a natural glucosyloxybenzyl 2-isobutylmalate, isolated fromBletilla striata, was reported with a prominent neuroprotective effect recently. The limited information on the metabolism of militarine impedes comprehension of its biological actions and pharmacology. This study aimed to investigate the metabolite profile and the distribution of militarine in vivo, which help to clarify the action mechanism further. A total of 71 metabolites (57 new metabolites) in rats were identified with a systematic method by ultra-high-performance liquid chromatography combined with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS/MS). The proposed metabolic pathways of militarine include hydrolyzation, oxidation, glycosylation, esterification, sulfation, glucuronidation and glycine conjugation. Militarine and its metabolites were distributed extensively in the treated rats. Notably, six metabolites of militarine were identified in cerebrospinal fluid (CSF), which were highly consistent with the metabolites after oral administration of gastrodin in rats. Among the metabolites in CSF, five of them were not reported before. It is the first systematic metabolic study of militarine in vivo, which is very helpful for better comprehension of the functions and the central nervous system (CNS) bioactivities of militarine. The findings will also provide an essential reference for the metabolism of other glucosylated benzyl esters of succinic, malic, tartaric and citric acids.Keywords:militarine;metabolite identification;metabolic profiles;UPLC-Q-TOF-MS/MS
研究领域:
药理学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2022
·
IF 4.52
Cuimin He,Weibin Huang,Xianmei Xue,Zhike Liang,Hao Ye,Kunping Li,Xujiang Yuan
Abrus precatorius leaves (APL) are one herb with the function of preventing and treating diabetes and widely used in health care and tea drinking in China. The objective of this study was to investigate the fingerprints, phytochemicals and quality evaluation of flavonoids from APL. Seven flavonoids were isolated and identified by NMR, ESI-MS and UV, with compounds 1–4, 6 from APL for the first time. An UPLC-ESI-Q-TOF/MS method was first established to evaluate the fingerprints. Similarity results showed that the overall quality of APL from different sources was relatively stable, but there were also some content differences, which could be used for regional classification. Total 29 compounds were identified by UPLC-MS/MS. An HPLC method was established to simultaneously determine the contents of seven flavonoids and could be used to identify and distinguish the quality of APL. The content of flavonoids in APL from different sources was 2.31–11.0%. This is the first report on the fingerprints, HPLC method and quality profile of seven flavonoids from APL.
研究领域:
植物化学
·
药物分析
✓ 已验证
产品关联
DOI
高影响因子
RSC Advances
·
2021
·Vol. 11
·期 37
·23002-23009
·
IF 3.361
Peng Jin,Kai Yang,Ruining Bai,Mei Chen,Shilin Yang,Kebo Fu,Jieli He
Microcystin-LR (MC-LR) generated by cyanobacteria is a kind of potent hepatotoxin, which poses a considerable threat to human health. In the research field of MC-LR removal, the quantitative analysis in a wide concentration range of samples is inevitable. In this paper, we presented the pseudo united use of an Ultra Performance Liquid Chromatography Mass Spectrometry (UPLC-MS) and High Performance Liquid Chromatography system with a Variable Wavelength Ultraviolet Detector (HPLC-VWD) approach to detect MC-LR. The UPLC-MS system was applied to determine MC-LR in trace concentration because of its high sensitivity. However, it is generally believed that the determination of high concentration samples by UPLC-MS will cause problems such as inaccurate quantification and contamination of ion sources. In consequence, the HPLC-VWD was employed to determine the high concentration of MC-LR. The sensitivity, precision and accuracy of the two methods were compared in detail. The linear ranges of UPLC-MS and HPLC-VWD methods were from 0.08 to 10 μg L−1 and 1 to 5000 μg L−1, respectively. The detection and quantification limits of UPLC-MS were 0.03–0.05 μg L−1 and 0.08 μg L−1, and the corresponding two values of HPLC-VWD were 0.6 and 1.0 μg L−1. The recoveries of UPLC-MS and HPLC-VWD were 88.5–106.7% and 98.7–101.6%, with the relative standard deviations of 3.72–5.45% and 0.38–1.69%, respectively. The potential adsorption properties of MC-LR on filter membranes with diverse materials and pore sizes were evaluated and the negative results were obtained. The detection of MC-LR by UPLC-MS was free from matrix effects. The presented UPLC-MS and HPLC-VWD methods were used to analyze the water samples from Erhai Lake, which is located in Dali, Yunnan, China. The results of UPLC-MS analysis indicated that the MC-LR was only identified in water samples of Shuanglang Bay and Xier River, with concentrations of 0.120 and 0.303 μg L−1, whereas MC-LR was not detected by HPLC-VWD.
研究领域:
环境科学
·
毒理学
·
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
危险品化学品经营许可证（带存储）