ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2018
·Vol. 410
·期 7
·2011-2018
·
IF 3.307
Yu Lingling,Wen Chao,Li Xing,Fang Shiqi,Yang Lichuan,Wang Tony,Hu Kaifeng
Quantification of endogenous and exogenous plasma glucose can help more comprehensively evaluate the glucose metabolic status. A ratio-based approach using isotope dilution liquid chromatography tandem mass spectrometry (ID LC-MS/MS) with indirect multiple reaction monitoring (MRM) of the derivative tag was developed to simultaneously quantify endo-/exogenous plasma glucose. Using diluted D-[ 13 C 6 ] glucose as tracer of exogenous glucose, 12 C 6 / 13 C 6 glucoses were first derivatized and then data were acquired in MRM mode. The metabolism of exogenous glucose can be tracked and the concentration ratio of endo/exo-genous glucose can be measured by calculating the endo-/exo-genous glucose concentrations from peak area ratio of specific daughter ions. Joint application of selective derivatization and MRM analysis not only improves the sensitivity but also minimizes the interference from the background of plasma, which warrants the accuracy and reproducibility. Good agreement between the theoretical and calculated concentration ratios was obtained with a linear correlation coefficient ( R ) of 0.9969 in the range of D-glucose from 0.5 to 20.0 mM, which covers the healthy and diabetic physiological scenarios. Satisfactory reproducibility was obtained by evaluation of the intra- and inter-day precisions with relative standard deviations (RSDs) less than 5.16%, and relative recoveries of 85.96 to 95.92% were obtained at low, medium, and high concentration, respectively. The method was successfully applied to simultaneous determination of the endo-/exogenous glucose concentration in plasma of non-diabetic and type II diabetic cynomolgus monkeys.
Graphical Abstract The scheme of the proposed ratio-based approach using isotope dilution LC-MS/MS with indirect MRM of the derivative tag for simultaneous quantification of endogenous and exogenous plasma glucose.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2025
·Vol. 48
·期 2
·e70100
·
IF 2.8
Liang Li,Rendan Zhou,Huiying Xie,Gang Li,Zhiguang Xu,Meijia Liu,Wanting Gao
The widespread use of organophosphorus pesticides (OPs) has raised significant environmental and health concerns due to their residues in soil and potential entry into the food chain. This study introduced chiral analysis methods for four OPs—methamidophos (METHP), dipterex (DIP), malathion (MALA), and isothiophos-methyl (ISOME)—using liquid chromatography–tandem mass spectrometry (LC–MS/MS) with cellulose-based chiral columns. Three distinct methods were established: one for METHP, another for DIP, and a third for MALA and ISOME. Key chromatographic variables, including organic mobile phases and column temperatures, were systematically optimized, achieving maximum resolutions ( R s) of 1.61 for METHP, 2.40 for DIP, 1.70 for MALA, and 2.02 for ISOME. The QuEChERS method was employed for sample pretreatment, ensuring high recoveries. All three methods demonstrated excellent linearity ( R > 0.998), accuracy with recoveries ranging from 79% to 121%, precision with RSD% < 11%, and sensitivity with low limits of enantiomer detection (LODs) as low as 0.17 µg/kg for METHP, 0.087 µg/kg for DIP, 0.062 µg/kg for MALA, and 0.054 µg/kg for ISOME, representing a sensitivity improvement of 16–172 times compared to existing methods. Field soil samples from Yangzizhou District, Nanchang, China, revealed significant contamination by ISOME, with concentrations of a single enantiomer reaching up to 8343 µg/kg, while MALA exhibited varying enantiomeric ratios with depth. This study provides robust analytical tools for monitoring chiral OP residues in soil, contributing to food safety and environmental protection.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Food Analytical Methods
·
2024
·
IF 2.6
Pan Xingyu,Chen Jinzi,Guo Tao,Kuang Fengjiao,Kang Zonghua,Luo Jianguang
Betel nut (Areca nut, AN) products are extensively consumed across East and South Asian countries, with Binglang being the predominant chewable AN product in China. Given the increased risk of carcinogenicity associated with alkaloid nitrogen oxides compared to the primary alkaloids in AN, this study aimed to establish a precise and sensitive method for quantitative analysis of the arecoline N-oxide (ACNO) and arecaidine N-oxide (ADNO) at three different processing stages of Binglang using liquid chromatography-tandem mass spectrometry (LC–MS/MS). The developed method underwent comprehensive validation, evaluating key analytical parameters including selectivity, linearity, sensitivity, accuracy, precision, and stability. Notably, the method demonstrated excellent sensitivity, with the limits of detection (LOD) ranging from 0.029 to 0.135 ng/mL, while the limits of quantification (LOQ) ranging from 0.095 to 0.450 ng/mL. Subsequently, the established analytical technique was applied to analyze 15 Binglang samples at three different processing stages, providing the first evidence of the content and variability of alkaloid nitrogen oxides throughout these stages. ACNO and ADNO were detected in all samples, and their total contents ranged from 4.31 to 32.82 μg/g. The changes observed across different processing stages indicated that the roasting process at 80 ℃ resulted in the promotion of alkaloid nitrogen oxides. This analytical approach constitutes a valuable tool for the quality control and risk assessment of Binglang and can be extended to other AN products, thereby assisting in addressing health concerns associated with these products.
✓ 已验证
产品关联
DOI
高影响因子
Analytical Methods
·
2025
·
IF 2.6
Jieting Zhang,Shuo Diao,Zhen Huang,Mengyuan Wu,Xintong Wang,Yiran Zhao,Mingming Yu,Xianzhen Wang,Jingchun Yao,Guimin Zhang,Sherwin K. B. Sy,Zhihua Lv,Hai Yang
Guided by the principles of Analytical Quality by Design (AQbD), a highly selective and sensitive LC-MS/MS method was established for the simultaneous quantification of 15 compounds in Shouhui Tongbian capsules, enabling their effective quality control. The separation was carried out on a BEH C18 column (1.7 μm, 2.1 × 100 mm) with a mobile phase comprising 0.1% formic acid in 3 mM ammonium acetate aqueous solution and methanol (60 : 40, v/v) at a flow rate of 0.30 mL min−1. The method exhibited good linearity within a certain concentration range (R2 > 0.9906) depending on the compound; the precision ranged from 0.6% to 14.7% and accuracy was within 11.2%. Among the 15 detected compounds, aloin had the highest content in the Shouhui Tongbian capsules, reaching 227.3780 mg g−1, followed by betaine and L-hydroxyproline, with concentrations of 1.3204 mg g−1 and 1.2929 mg g−1, respectively. This method simultaneously detected the content of 15 compounds in five batches of Shouhui Tongbian capsules.
研究领域:
分析化学
·
药物分析
·
质量控制
·
色谱-质谱分析
·
中医药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2017
·
IF 3.255
Katerina Grigori,Yannis L. Loukas,Anđelija Malenović,Vicky Samara,Anastasia Kalaskani,Efi Dimovasili,Magda Kalovidouri,Yannis Dotsikas
A sensitive Liquid Chromatography tandem mass spectrometry (LC–MS/MS) method was developed and validated for the quantitative analysis of three potential genotoxic impurities (318BP, M9, S5) in meropenem Active Pharmaceutical Ingredient (API). Due to the requirement for LOD values in ppb range, a high concentration of meropenem API (30 mg/mL) had to be injected. Therefore, efficient determination of meropenem from its impurities became a critical aim of this study, in order to divert meropenem to waste, via a switching valve. After the selection of the important factors affecting analytes’ elution, a Box-Behnken design was utilized to set the plan of experiments conducted with UV detector. As responses, the separation factor s between the last eluting impurity and meropenem, as well as meropenem retention factor k were used. Grid point search methodology was implemented aiming to obtain the optimal conditions that simultaneously comply to the conflicted criteria. Optimal mobile phase consisted of ACN, methanol and 0.09% HCOOH at a ratio 71/3.5/15.5 v/v. All impurities and internal standard omeprazole were eluted before 7.5 min and at 8.0 min the eluents were directed to waste. The protocol was transferred to LC–MS/MS and validated according to ICH guidelines.
研究领域:
分析化学
·
药物分析
·
药学
✓ 已验证
DOI
PubMed
高影响因子
Scientific Reports
·
2017
·
IF 4.259
Cong Xie,Tong-Meng Yan,Jia-Mei Chen,Xiao-Yan Li,Juan Zou,Li-Jun Zhu,Lin-Lin Lu,Ying Wang,Fu-Yuan Zhou,Zhong-Qiu Liu,Ming Hu
This study aims to determine whether enzyme activities are correlated with protein amounts and mRNA expression levels of five major human sulfotransferase (SULT) enzymes in 10 matched pericarcinomatous and hepatocellular carcinoma liver samples. The MRM UHPLC-MS/MS method, Western blot and RT-PCR were used along with SULT activity measurement using probe substrates. The LC-MS/MS method was specific for all five tested SULTs, whereas Western blot was specific for only two isoforms. The activities of SULT1A1, SULT1B1, SULT1E1 and SULT2A1 in 9 of 10 samples showed a significant decrease in tumor tissues relative to matched pericarcinomatous tissues, whereas the activities of SULT1A3 in 7 of 10 samples increased. The turnover numbers of SULTs did not change, except for SULT1A1. A generally high degree of correlations was observed between SULT activities and protein amounts (r 2 ≥ 0.59 except one), whereas a low degree of correlations was observed between SULT activities and mRNA expression levels (r 2 ≤ 0.48 except one). HCC reduced the SULT activities via impaired protein amounts. LC-MS/MS quantification of SULTs is highly reliable measurement of SULT activities, and may be adopted for implementing precision medicine with respect to drugs mainly metabolized by SULTs in healthy and HCC patients.
研究领域:
药理学
·
分子生物学
·
肿瘤学
·
临床化学
✓ 已验证
DOI
PubMed
高影响因子
TALANTA
·
2026
·
IF 6.7
Feng Chen,Ziwei Deng,Yueping Jiang,Yayun Tan,Xiaoxia Yang,Huanhuan Li,Wendan Zhang,Xiangjin Shu,Aimin Wang,Chengfeng Qiu
Therapeutic drug monitoring (TDM) is essential for optimizing antimicrobial therapy and curbing resistance, yet conventional venipuncture limits its widespread application due to invasiveness and operational complexity. This study aimed to establish a rapid LC-MS/MS method for simultaneous quantification of 12 antimicrobial agents and to evaluate the feasibility of using fingertip capillary serum as an alternative to venous serum for TDM. A liquid chromatography tandem mass spectrometry method was developed and validated for the simultaneous quantification of vancomycin, linezolid, voriconazole, sulfamethoxazole, trimethoprim, piperacillin, cefoperazone, ceftazidime, ceftobiprole, meropenem, imipenem, and cilastatin in human serum. The method was applied to analyze 379 paired clinical samples (fingertip serum versus venous serum), and agreement between the two sampling approaches was assessed using Deming regression and Bland Altman analysis. The method required only 10 μL of serum and a total run time of 4 min. Deming regression slopes ranged from 0.910 to 1.017. Bland Altman analysis showed that 100.0% of the data points fell within ±20.0% limits of agreement for all antibiotics except vancomycin (96.7%) and cilastatin (97.5%). This study provides large scale clinical evidence demonstrating high concordance between fingertip serum and venous serum concentrations for 12 antimicrobial agents. By directly obtaining serum, this approach fundamentally avoids the hematocrit effect and matrix conversion issues inherent in whole blood microsampling, offering a minimally invasive TDM strategy fully aligned with the gold standard matrix. This strategy is particularly suitable for special populations such as children, the elderly, and critically ill patients.
✓ 已验证
DOI
PubMed
高影响因子
FOOD RESEARCH INTERNATIONAL
·
2026
·
IF 8.8
Mengyao Zhang,Tianyi Tao,Zixuan Wang,Shijie Ding,Guanghong Zhou,Chong Wang
Cultured meat presents significant potential as a sustainable supplement to traditional livestock farming. Addressing the critical challenge of residual chemical substances from the culture media, this study established a rapid method combining protein precipitation (PP) with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the quantitative analysis of 12 risk substances in both porcine cultured meat biomass and washing solutions. All validation parameters, including linearity, sensitivity, precision, accuracy, recovery, matrix effect, dilution integrity and stability, met the predefined acceptance criteria. The results demonstrated that consecutive centrifugal washing cycles significantly reduced residue levels in porcine cultured meat biomass, with the majority of the 12 target substances effectively removed after four cycles. Analysis of 15 production batches revealed that 9 out of the 12 target substances were below the limit of detection (LOD) in the final product. For the remaining three substances, the mean concentrations were 307.91 μg/kg for forskolin, 568.04 μg/kg for thymidine, and 397.61 μg/kg for N -acetylcysteine. A target hazard quotient (THQ) assessment confirmed that none of the 12 residues posed a health risk. These findings provide the technical groundwork and theoretical rationale needed to optimize quality and safety specifications in the cultured meat industry.
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Jinlin He,Luying Shen,Dunming Xu,Ting Sun,Yan Chen,Jinsheng Hu,Yan Ji,Lijuan Yan
First demonstration of C18-column HILIC-like separation for aminoglycosides. • Hydrophilic retention via water layer & vicinal silanols on base-deactivated silica. • Tandem WCX-C18 SPE protocol developed for effective matrix cleanup. • Robust, MS-compatible, practical monitoring of aminoglycoside residues in foods. An LC–MS/MS method was developed for the simultaneous determination of 16 aminoglycosides (AGs) in pork, chicken, milk, and eggs using a conventional Hypersil base-deactivated silica (BDS) C 18 column operated under HILIC-like conditions. Unlike typical C 18 -based methods that rely on ion-pairing reagents in the LC mobile phase, separation was achieved with an ion-pair-free mobile phase consisting only of 0.1% formic acid and acetonitrile under gradient elution. Column comparison, aqueous-fraction experiments, and SRM 870 probe testing indicated a mixed retention mechanism involving hydrophilic partitioning into a water-enriched interfacial layer and reversible interactions with accessible residual silanol sites. Because the method prioritizes MS compatibility and reproducible multi-residue quantification, compound-specific MRM transitions and matrix-matched calibration were used to ensure selectivity and quantitative reliability. The method showed good linearity (R² > 0.99), satisfactory accuracy (71.2–99.8%) with reported standard deviations, acceptable precision (CV ≤ 11.3%), and low detection limits (LODs 3–15 μg/kg; LOQs 10–50 μg/kg). Overall, this work demonstrates that a conventional C 18 column can exhibit pronounced hydrophilic selectivity under high-organic conditions, offering a practical, MS-friendly alternative for aminoglycoside residue analysis and informing future stationary-phase development for hydrophilic separations.
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF ETHNOPHARMACOLOGY
·
2026
·
IF 6.8
Hongrui Ma,Xin Ding,Junli Liang,Ping Li,Runuo Wang,Ya Zhang,Guangguo Tan
Ethnopharmacological relevance Aconiti Lateralis Radix Praeparata (Fuzi in Chinese) is an herbal medicine for restoring yang from collapse. However, the multiregional neurotoxicity of Fuzi was unclear. Aim of the study This work was designed to discover the multiregional neurotoxicity-associated metabolic alterations induced by Fuzi in brain of rat. Materials and methods Fuzi-distributed components in cerebrospinal fluid and multiple brain regions were analyzed by using ultra-high performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UHPLC-QTOF-MS). The multiregional neurotoxicity including hippocampus, striatum and cerebellum was evaluated by behavioral tests, biochemical examinations, Hematoxylin/eosin (H&E), Nissl staining, TUNEL staining, reactive oxygen species and metabolomic analyses. Both cerebrospinal fluid metabolomics and the multiregional target tissue (hippocampus, striatum and cerebellum) metabolomics of the brain, based on UHPLC-QTOF-MS, were conducted to reveal the metabolic changes associated with Fuzi neurotoxicity. Results 13, 11, 11 and 8 ingredients of Fuzi were distributed into the cerebrospinal fluid, hippocampus, striatum, and cerebellum, respectively. Fuzi exposure could cause motor dysfunction and anxiety-like behaviors and decrease the level of brain derived neurotrophic factor (BDNF) and increase the level of neuron specific enolase (NSE). Fuzi exposure produced oxidative stress, neuronal lesions, neuronal apoptosis and metabolic alterations, which produced the multiregional neurotoxicity in the brain. The differentially expressed metabolites associated with Fuzi exposure in the cerebrospinal fluid, hippocampus, striatum and cerebellum predominantly involved glycerophospholipid metabolism, sphingomyelin metabolism, arachidonic acid metabolism, purine metabolism, amino acid metabolism, TCA cycle and fatty acid β-oxidation. Conclusion Fuzi exposure produced the multiregional neurotoxicity in the hippocampus, striatum and cerebellum of the brain.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2023
·Vol. 28
·期 5
·2377
·
IF 4.6
Zili Guo,Bianbian Gao,Miaoliang Fan,Lisha Chen,Changjun Zhang,Xianrui Liang,Weike Su,Yuanyuan Xie
XYY-CP1106, a candidate compound synthesized from a hybrid of hydroxypyridinone and coumarin, has been shown to be remarkably effective in treating Alzheimer’s disease. A simple, rapid and accurate high-performance liquid chromatography coupled with the triple quadrupole mass spectrometer (LC-MS/MS) method was established in this study to elucidate the pharmacokinetics of XYY-CP1106 after oral and intravenous administration in rats. XYY-CP1106 was shown to be rapidly absorbed into the blood (Tmax, 0.57–0.93 h) and then eliminated slowly (T1/2, 8.26–10.06 h). Oral bioavailability of XYY-CP1106 was (10.70 ± 1.72)%. XYY-CP1106 could pass through the blood–brain barrier with a high content of (500.52 ± 260.12) ng/g at 2 h in brain tissue. The excretion results showed that XYY-CP1106 was mainly excreted through feces, with an average total excretion rate of (31.14 ± 0.05)% in 72 h. In conclusion, the absorption, distribution and excretion of XYY-CP1106 in rats provided a theoretical basis for subsequent preclinical studies.Keywords:XYY-CP1106;Alzheimer’s disease;LC-MS/MS;pharmacokinetics;tissue distribution;excretion study
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2023
·
IF 8.8
Xin Fang,Yanan Liu,Jingyi Xiao,Cunqiang Ma,Youyi Huang
High-performance liquid chromatography (HPLC), headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC–MS) and ultra-high performance liquid chromatography–Q-Exactive HF-X mass spectrometer (UHPLC–Q-Exactive HF/MS) were carried out to reveal dynamic changes of volatile and non-volatile compounds during the withering process of black tea. A total of 118 volatile organic compounds (VOCs) and 648 metabolites were identified in fresh and withered tea-leaves, respectively. Among them, 47 VOCs (OAV > 1.0) for the aroma formation, and 46 characteristic metabolites (VIP > 1.50, p < 0.01) selected through orthonormal partial least squares-discriminant analysis, indicated the withering contribution during black tea processing. Overall, the withering promoted alcohols, aldehydes, phenols, heterocyclic oxygen, hydrocarbons and halogenated hydrocarbons through relevant hydrolyzation, decomposition, terpene synthesis, and O -methylation. The hydrolyzation, O -methylation, condensation and N -acylation of kaempferol glycosides, quercetin glycosides, ester catechins, and gallic acid generated the accumulation of methoxyl flavonoids and flavonoid glucosides, dihydrokaempferol, syringic acid, theaflavins, and N -acylated amino acids, respectively.
✓ 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）