MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Yongyin Zhou,Hui Li,Hongjun Luo,Zhexuan Lin,Wenhong Luo
An untargeted UHPLC-MS method was developed for the preliminary screening of differential amino acids between two mouse brain tissue samples, and a targeted UHPLC-MS/MS method was developed for the quantitative determination of amino acids in mouse brain tissue samples. The sample processing procedure, chromatographic conditions and MS parameters were optimized. The mouse brain tissue samples were homogenized with HCl solution (0.01 mol/L), protein precipitated with methanol and centrifugation. For the untargeted method, one sample was derivatized with butanol (D0) and another sample was derivatized with deuterated butanol (D9), then combined together and analyzed with UHPLC-MS. Chromatographic peak area ratio for each amino acid was then used for differential analyses between two samples. Results showed good accuracy with standard spiked samples (83.4–113.0 %). For the targeted quantitative method, the sample supernatants were dried and residues were derivatized with butanol (D0). Internal standards of amino acids derivatized with deuterated butanol (D9) were added before analyzed with UHPLC-MS/MS. The intra- and inter-day precisions were in the intervals of 0.5–8.1 % and 0.3–9.1 %. The LOD and the LOQ were ranged from 0.03 × 10 −3 to 0.92 × 10 −3 µg mL −1 and 0.08 × 10 −3 to 3.08 × 10 −3 µg mL −1 , respectively. Spiked recoveries were from 96.8 % to 111.7 %. Both methods were applied to analyze amino acids in brain tissue of C57BL/6 mice treated and untreated with piperine and the result showed that the levels of glutamic acid, aspartic acid, histidine, asparagine, γ-aminobutyric acid, alanine, leucine and isoleucine significantly decreased in the piperine treated group comparing with the untreated group.
研究领域:
分析化学
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神经生物学
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药理学
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产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Xiaoqian Chen,Luyao Yu,Yingxia Guo,Jiansong You,Meiyun Shi,Yalin Xi,Lei Yin
An analytical assay based on ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) technique for absolute quantification of vancomycin in complexed biological matrix was developed in this study. Reversed phase column with gradient elution was chosen for chromatographic separation of vancomycin and internal standard (IS) norancomycin. Sample pretreatment was performed by micro-solid phase extraction (μ-SPE) with Oasis® MAX μElution Plate (I.D., 30 μm). Multiple reaction monitoring (MRM) transition was chosen for monitoring of the analytes. For vancomycin, mass-to-charge ratio ( m/z ) of the MRM transition was 725.3→144.1; For norvancomycin, m/z of the MRM transition was 718.3→144.2. The running time was 3 minutes for each sample. The UHPLC-MS/MS method showed a good linear relationship (R 2 ≥0.995) in the concentration range of 0.5–100 μg/mL. The intra- and inter-day accuracies (relative error, RE) are within the range of −3.44 %-1.50 % and precisions are between 3.48 % and 10.19 %. μ-SPE could enrich the analytes and decrease the endogenous interferences, thereby improving the selectivity and sensitivity of the method. The analytical assay is selective, accurate and reproducible. The assay was successfully applied to therapeutic drug monitoring of vancomycin in clinical application.
研究领域:
临床医学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Food Chemistry-X
·
2024
·
IF 6.5
Shaowei Li,Yuting Yuan,Liangxiao Zhang,Fei Ma,Peiwu Li
This study was based on QuEChERS cleanup coupled with UHPLC-MS/MS for the determination of γ-oryzanol compounds in vegetable oils. Several parameters of QuEChERS and UHPLC-MS/MS were studied for purification and detection of γ-oryzanol compounds in oil samples. Under the optimized conditions, the whole pretreatment procedure could be accomplished within 10 min without tedious procedure, larger volume of organic solvent and complicated apparatus. The limit of detections and the limit of quantifications for γ-oryzanol compounds were ranging from 0.1-0.3 µg kg −1 and 0.4–1.0 µg kg −1 , respectively. Satisfactory recoveries of all analyts were ranging from 72.2 % to 101.3 %, and the intra-day and inter-day precision were less than 10.6 %. The validation indicated that rice band oil and corn oil were rich in 24-mCAF, CAF, β-SIF, CMF and STF. The QuEChERS-UHPLC-MS/MS simultaneously quantified five γ-oryzanol compounds in lipid matrices and assessed the nutritional and functional substances of vegetable oils.
研究领域:
食品科学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2013
·
IF 2.947
Fengtao Li,Jin-ao Duan,Dawei Qian,Sheng Guo,Yuhua Ding,Xunhong Liu,Yefei Qian,Yunru Peng,Yijun Ren,Yu Chen
A rapid and sensitive hydrophilic interaction liquid chromatography method was developed for the identification and quantitative determination of 17 nucleosides and nucleobases by using ultra-high performance liquid chromatography separation system coupled to triple quadrupole mass spectrometer. Sufficient separation of the target compounds was achieved on an Acquity BEH Amide column (2.1 mm × 100 mm, 1.7 μm) in a single run of 9 min. The LOD and LOQ were in the range of 0.017–50.00 ng ml −1 and 0.056–146.00 ng ml −1 , respectively. Then, the method was applied for the analysis of nucleosides and nucleobases in Elaphuri Davidiani Cornu and Cervi Cornu . Multivariate statistical analysis was also used to investigate the differences in the nucleosides and nucleobases profiles among the samples. The present study also provided helpful information for quality control of Elaphuri Davidiani Cornu and Cervi Cornu .
研究领域:
分析化学
·
药学
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Yingxia Guo,Meichen Liu,Yajie Cheng,Jiye Tian,Chunpeng Feng,Qingbin Wang,Xuan Zhao,Lei Yin
Methoxy-polyethylene glycol amine (mPEG-NH₂), an important pharmaceutical excipient, has been extensively utilized in the field of biomedicine. To advance the development of mPEG-NH₂-related drug delivery systems, it is crucial to understand the safety profile and cellular pharmacokinetic behavior of mPEG-NH₂ polymers. In this study, a straightforward analytical assay based on ultra-high performance liquid chromatography and tandem mass spectrometry (UHPLC-MS/MS) for quantifying mPEG 5 -NH₂ in biological matrices was established and validated. Multiple reaction monitoring (MRM) transitions were selected for quantification of mPEG 5 -NH₂ (mass-to-charge ratio, m/z 252.1 → 87.7) and octaethylene glycol (OH-PEG 8 -OH) (mass-to-charge ratio, m/z 371.2 → 89.2). The UHPLC-MS/MS assay demonstrated excellent linearity within the concentration range of 0.01–10 μg/mL, with an R² value of 0.9996. Both intra-day and inter-day accuracies and precisions of the analytical method were within ± 9.19 %. This analytical assay was successfully applied to study the in vitro cellular toxicity and uptake behavior of mPEG 5 -NH₂ in MCF-7 cells. The results indicate that high doses of mPEG 5 -NH₂ may have potential toxicity to MCF-7 cells.
研究领域:
药物分析
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毒理学
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生物医学工程
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产品关联
DOI
PubMed
高影响因子
EUROPEAN FOOD RESEARCH AND TECHNOLOGY
·
2023
·Vol. 249
·期 4
·1137-1146
·
IF 3.3
Zhu Yan,Di Lei,Cheng Shengyu,Jin Yueying,Zhang Minghui,Zhang Lingli,Wang Xin,Li Xi-Ling,Han Yu,Xu Chun-Yan,Min Jun Zhe
A novel UHPLC–MS/MS method with high sensitivity and selectivity for simultaneous detection and chiral resolution of DL-amino acids in beer was established using the newly developed mass spectrometry probe (S)-(3-(4-carboxythiazolidin-3-yl)-3-oxopropyl) diphenylsulfonium (CTOD). The gradient analysis of five chiral amino acids (DL-Asp, DL-Glu, DL-Ala, DL-Pro, and DL-Phe) was carried out on a BEH C18 (2.1 × 150 mm, 1.7 μm) for 30 min with a mobile phase of 0.1% formic acid aqueous solution and 0.1% formic acid methanol/acetonitrile (7:3) solution. The resolutions of DL-amino acids ranged from 1.71 to 5.42. The correlation coefficients were ≥ 0.9994 in the range of 0.25 to 1200 pmol. Meanwhile, limits of detection (LOD) and limits of quantitative (LOQ) analysis were 0.05–0.25 pmol and 0.13–0.50 pmol, respectively. Furthermore, the intra-day and inter-day precision ranged from 0.34% to 6.31%, and the average recoveries ranged from 97.50% to 107.50%. The method was applied to the quantitative analysis and comparison of DL-amino acids in beer samples from 10 different manufacturers, and it was found that the beers were rich in D-amino acids. Four D-AAs including D-Ala, D-Pro, D-Glu, D-Phe (1.9–29.8 μmol L −1 ) and five L-AAs including L-Pro, L-Ala, L-Phe, L-Glu, L-Asp (5.3–2315.9 μmol L −1 ) were detected in the beer samples. The average content of L-AAs in the 10 beer samples was significantly higher than that of D-AAs. This study provides a new method for detecting chiral amino acids in beer and reliable data for evaluating the nutritional value of beer.
Graphical abstract
研究领域:
分析化学
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食品科学
·
营养学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY
·
2020
·
IF 3.255
Jingwen Hu,Shi-En Chen,Shuyun Zhu,Wenhui Jia,Jing Sun,Xian-En Zhao,Huwei Liu
In this work, a new series of chemical isotope labeling reagents, levofloxacin-hydrazide-based mass tags (LHMTs) named as LHMT359/360/361/362/363/364/365/366/373/375/376/378/379/381 were first designed and synthesized for the high-throughput analysis of potential biomarkers containing hexanal and heptanal of lung cancer. We exploited a new core structure of levofloxacin-d3, which significantly enhanced the multiplexing capability. Among them, LHMT359 was used for labeling standard compounds as internal standards for quantification. Using LHMT373-heptanal as dummy template, dummy magnetic molecularly imprinted polymers (DMMIPs) were prepared for magnetic dispersive solid-phase extraction after derivatization procedure. Other 12 LHMTs were established for high-throughput labeling hexanal and heptanal in human serum samples. The presynthesized DMMIPs can selectively extract LHMTs-derivatives of hexanal and heptanal from equally mixed derivatization solutions. The enriched derivatives of hexanal and heptanal were quantified by ultrahigh-performance liquid chromatography tandem mass spectrometry (UHPLC–MS/MS). A single UHPLC–MS/MS run enabled simultaneously quantifying hexanal and heptanal from 12 serum samples only within 2 min. The limits of detection were all 0.5 pM for hexanal and heptanal. The accuracies from human serum samples ranged from −10.2% to +11.0% with the intra- and interday precisions less than 11.3%. Meanwhile, this method was successfully applied for the analysis of hexanal and heptanal in serum samples from healthy people and lung cancer patients. The results show that this method has the significant advantages of high sensitivity, accuracy, selectivity, and analysis-throughput. The method application indicates that the developed method is promising in the screening of suspected lung cancer patients.
研究领域:
分析化学
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医学
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生物标志物研究
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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
·
2021
·
IF 3.205
Tao Hu,Xinyu Ge,Junyang Wang,Ning Zhang,Xingxing Diao,Lihong Hu,Xiachang Wang
Iridin, one of the main bioactive components isolated from Belamcanda chinensis (L.) DC, exerts various pharmacological activities, such as anti-inflammation, antioxidant, and antitumor. However, the metabolism and pharmacokinetics of iridin are still unknown. After 100 mg/kg administration of iridin orally, the plasma, urine, and fecal bio-samples from Sprague–Dawley (SD) rats were collected and detected by ultrahigh-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). The pharmacokinetics of the major metabolite irigenin (aglycon of iridin) and a total of thirteen metabolites of iridin were identified, including five metabolites in plasma, ten metabolites in urine, and six metabolites in feces. The most principal metabolic pathway of iridin was glucuronidation after demethylation and was mediated by UDP-glucuronosyltransferases (UGTs) 1A7, 1A8, 1A9 and 1A10. This study highlights the first-time investigation of the metabolism of iridin in vivo, and the pharmacokinetics of irigenin (the major metabolite of iridin) in rats. These results provide robust evidence for further research and clinical application of iridin.
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
JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2022
·
IF 1.467
An-ping Li,Yan-ping Shi
Farfarae Flos, a frequently used traditional herbal medicine with outstanding antitussive and anti-asthmatic effects. As an herbal rich in natural flavonoids, the quantitative determination of multi-flavonoids can be helpful to comprehensively evaluate its quality. Herein, an efficient, sensitive and accurate UHPLC-MS/MS method was established to simultaneous determinate nine flavonoids (rutin, hyperin, kaempferol-3-O-rutinoside, hesperidin, luteolin, quercetin, kaempferol, apigenin, and genkwanin) in Farfarae Flos. The calibration curves of the analytes had good linearity (R2 ≥ 0.9991). Limit of detection and limit of quantitation of each analytes was in the range of 1.06 × 10−5–2.26 × 10−3 μg·mL−1 and 3.52 × 10−5–7.53 × 10−3 μg·mL−1. The relative standard deviation (RSD) of the intra-day and inter-day precision was less than 2.71% and 2.94%. The RSD of repeatability test and stability test was less than 2.35% and 2.56%. The recovery rates were in the range of 95.27%–103.60%. The method was further applied to determinate 40 batches of samples that derived from different plant parts and with definite habitat. The results of chemometric statistical analysis showed that, firstly, the content of flavonoids can effectively reflect the differences between traditional medicinal parts and impurities. Secondly, the geographical environment has impact on the quality. In conclusion, this study provides a valuable methodological reference for the quality evaluation and further resource utilization of Farfarae Flos.
研究领域:
药学
·
分析化学
·
植物学
✓ 已验证
DOI
高影响因子
Bioanalysis
·
2016
·Vol. 8
·期 13
·
IF 2.813
Qinghua Wang,Yan Wen,Tianyi Xia,Xiaojuan Xiong,Shouhong Gao,Chunhua You,Xia Tao,Feng Zhang,Wansheng Chen
Aim: Quantification of amino acids in human plasma has become an important and essential analysis parameter in life science. In this paper, we developed a targeted UHPLC–MS/MS method for 18 amino acids in the renal transplant patients. Methods & results: Plasma in small volume (150 μl) was pretreated by a one-step protein precipitant extraction for analysis. Detection was executed by MS/MS in the MRM mode. Assays were validated according to current bioanalytical guidelines, with good linearity (R > 0.99), intraday and interday precision (CV < 11.6%, RE ≤ ± 14.8%), extraction recovery (between 77.4 and 117.6%), matrix effect (73.3–118.0%) and stability (RE≤ ±14.7%). Conclusion: The method was successfully applicable for amino acid analysis in the renal transplant patient.
研究领域:
生物分析
·
医学检测
·
临床化学
✓ 已验证
DOI
PubMed
高影响因子
Drug Design Development and Therapy
·
2020
·
IF 3.216
Xiaofang Jiang,Lin Zhou,Lihua Zuo,Xiaohui Wang,Yingying Shi,Xiangyu Du,Jun Zhang,Liwei Liu,Zhuolun Li,Lianping Xue,Xin Liu,Zhi Sun
Purpose Shenkang injection, a traditional Chinese herbal prescription, had been widely used in renal disease due to its perfect curative effect. In this research, a novel, sensitive, accurate and rapid liquid chromatography-tandem mass spectrometric method was developed to simultaneously detect the seven active ingredients in rat plasma of Shenkang injection and investigate its pharmacokinetic behaviors with metabolism profiling meanwhile.Methods For accurate pharmacokinetic quantitation, a WATERS ACQUITY UPLC® BEH C18 column was used to perform a separation and acetonitrile-water (0.1% formic acid) was selected as mobile phase for gradient elution with a flow rate of 0.20 mL/min. A heated electrospray ionization with selective reaction monitoring mode was used to monitor the precursor-product ion transitions for all the analytes and IS.Results They all showed good linearity over a wide concentration range (r>0.996 3) and the lower limit of quantification (LLOQ) was 0.1–1.0 ng/mL for analytes. The validation parameters were all within the acceptable limits. Furthermore, for metabolism profiling study, metabolites of the seven ingredients were identified from the rat plasma based on the accurate mass and fragment ions. The metabolic pathways mainly focus on reduction, dehydration and conjugation.Conclusion This study provided an overview of disposition of Shenkang injection, which is highly instructive for better understanding the effectiveness and toxicity of this drug.
研究领域:
中药学
·
药理学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Yu Tang,Zhe Wang,Menglin Li,Ruiping Zhang,Jinlan Zhang
A rapid, sensitive and wide coverage ultra-high-performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) method has been developed and validated for the simultaneous quantitation of 14 alkylation DNA adducts in cell genomic DNA, RNA and cell contents isolated from the in vitro cultured human kidney cell line 293 T and the human liver cell line L02 exposed to 3 genotoxic reagents: N -methyl -N- nitrosourea (MNU), methyl methanesulfonate (MMS) and 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK). After exposure, DNA was isolated and directly hydrolysed under acid conditions or digested by enzymes to obtain the hydrolysates containing DNA alkylation adducts followed by optimization of the pretreatment method and chromatographic separation conditions. Quantification was performed on a Waters ACQUITY UPLC BEH Amide column (1.7 μm, 2.1 × 150 mm) using an electrospray ionization (ESI) source in positive mode by selective reaction monitoring (SRM) at the precursor to product ion transitions of 14 analytes. The method showed selectivity, good linearity (r＞0.9950), accuracy (82.1%–115%), and intra-day (RSD%＜14%) and inter-day (RSD%＜15%) precision for 14 analytes. The recoveries of two pretreatment methods were all more than 50.5%, and no relative matrix effects were observed. Additionally, the samples were stable after short-term storage at 20 ℃ for 2 h, at 4 ℃ for 48 h or one cycle of freeze-thaw at −80 ℃. The established UHPLC-MS/MS method was used to evaluate the changes in alkylation DNA adducts and epigenetic modification-related methylcytosine after exposure to genotoxic reagents. For the first time, the results demonstrated that 3 genotoxic reagents induced different total amounts of adducts in the following sequence: MMS ＞ NNK ＞ MNU, and showed significant differences in the ratios of 7MeG to 1MeA and 1MeG to 1MeA in the 293 T cell model. Meanwhile, 293 T and L02 cells revealed significantly different DNA adduct formation characteristics in the contents of 1MeG and 1MeA. The DNA adduct formation relationships between DNA, RNA, and cell contents were probed to predict cancer risk and potential genotoxic exposure. This approach could be used to investigate the DNA adducts, their formation and the relationship to the mutagenicity or carcinogenicity of genotoxic reagents in future studies.
研究领域:
毒理学
·
分析化学
·
分子生物学
✓ 已验证
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）