JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2017
·
IF 3.255
Yuan Wang,Qing Li,Yue Dai,Ronghua Pan,Yufeng Xia
A specific and sensitive LC–MS/MS method was established for the simultaneous determination of bergenin, protocatechuic acid and gallic acid, the main active constituents of Saxifraga stolonifera (L.) Meerb. herb, in rat plasma. After fully validated, the method was applied to the comparative pharmacokinetic studies of the three compounds orally administered alone and in combination in the S. stolonifera extract, respectively. The results showed that the pharmacokinetic parameters, including C max , T max , AUC, CL z /F, MRT 0-∞ , were significantly different for both bergenin and protocatechuic acid in the extract as compared to the corresponding compounds administered alone. However, the pharmacokinetic behavior of gallic acid in the extract did not differ from that administered alone. Further studies found that quercetin, coexisting in the herb extract, significantly decreased the glucuronidation of bergenin through inhibiting the activities of UGT1A1 and UGT1A3, and reduced the metabolism of protocatechuic acid by inhibiting the activity of catechol-O-methyltransferase. Quercetin and other flavonoids occurring in the S. stolonifera extract might increase the absorption and improve the bioavailability of bergenin and protocatechuic acid by slowing down the liver metabolism. The findings provide a good guidance for the development and clinical application of S. stolonifera .
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JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Yang Yang,Jin Wang,Jia Qiu,Yan Luo,Chun Yang,Shali Tang,Hui Cao,Qian Wang,Xiaojing Lai
To monitor per- and polyfluoroalkyl substances (PFAS) in food contact materials (FCMs), an LC-MS/MS method for the simultaneous detection of 35 PFAS was developed and validated in paper and plastic products. Chromatographic and mass spectrometry parameters, extraction solvents, matrix effects in details were studied. The impact of matrix effects on PFAS concentration was analyzed, revealing that the matrix enhancement effect was more significant for some PFAS with low concentrations. In order to eliminate the matrix effect and enhance detection accuracy, a straightforward pretreatment method combining methanol ultrasonic extraction with dispersive solid-phase extraction (d-SPE) was established. PFHpA, PFDA, PFTriDA, PFTeDA, PF-3,7-DMOA, HFPO-DA, PFHxS, PFHpS, PFOS, 4:2 FTS, 6:2 FTS, 8:2 FTS, 10:2 FTS, and 6:2 diPAP required further d-SPE extraction with PSA, and other substances could be directly extracted by methanol ultrasonic treatment. The recoveries of the established method for all compounds ranged from 62.40 to 135.80%, with a relative standard deviation (RSD) of 0.15% to 16.81%. The limit of quantitation was between 0.005 and 0.02 mg·kg −1 . The method was applied to detect PFAS in 119 FCMs, resulting in the identification of 15 PFAS.
研究领域:
分析化学
·
食品安全
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2025
·
IF 3.8
Li Wenya,Gao Bingling,Yang Tao,Tang Liping,Song Dan,Li Hongmei,Sun Keqi,Xiao Peng
3,3′,5-Triiodothyronine (T3) plays a crucial role in the diagnosis and evaluation of thyroid diseases. The current reference measurement procedure (RMP) has been in place for 20 years and is widely adopted by reference laboratories around the world. To enhance the performance of the RMP, we developed and validated a simplified, SI-traceable candidate RMP specifically targeting serum total T3 (TT3) using isotope dilution-liquid chromatography with tandem mass spectrometry (ID-LC–MS/MS). Specifically, T3 reference material was employed as the standard. Compared to the RMP, our method incorporates a simplified serum cleanup process involving protein precipitation and nitrogen drying. The method validation followed ISO guidelines for measurement uncertainty assessment. Our results indicated that there was no significant conversion of T4 into metabolites during the serum pretreatment. The lower limit of the measuring interval was determined to be 0.077 nmol/L, and the regression model was linear across a range of 0.016 to 13.086 nmol/L. The imprecision of intra-assays ranged from 0.1 to 1.9%, while inter-assay imprecision ranged from 0.5 to 1.2%. The bias observed when analyzing SRM971 was between − 0.34 and − 1.65%. This candidate RMP demonstrated excellent agreement with the RMPs developed by RELA activity, showing a mean bias falling within the educational mean ratio (6%). The measurement uncertainties were 0.022 nmol/L for RELA2023A and 0.120 nmol/L for RELA2023B. In conclusion, the developed candidate RMP is traceable, reliable, and easy to operate, showing promising potential for the development of serum reference materials and the standardization of routine assays. Graphical
研究领域:
临床检验学
·
内分泌学
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JOURNAL OF SEPARATION SCIENCE
·
2019
·Vol. 42
·期 16
·2592-2601
·
IF 2.516
Hongmin Zhang,Xintong Hu,Miao Qiao,Yang Li,Shijie Cao,Liqin Ding,Xinchi Feng,Ning Kang,Deqin Zhang,Feng Qiu
A rapid and sensitive liquid chromatography with tandem mass spectrometry method was developed and validated for simultaneous determination of puerarin, daidzin, daidzein, 3′-hydroxy puerarin, and genistein in rat plasma after oral administration of Puerariae lobatae radix extract. The method of protein precipitation with acetonitrile was used for sample preparation. Chromatographic separation was achieved on a C 18 column with the mobile phases of acetonitrile/water containing 0.1% formic acid. The analytes were detected by mass spectrometer with an electrospray ionization source operating in the negative ion mode. The linearity, precision, accuracy, dilution reliability, recovery, matrix effects, and stability of the method were within acceptable ranges. The developed method was successfully used to compare the pharmacokinetic characteristics of five analytes in normal and type 2 diabetics rats after oral administration of Puerariae lobatae radix extract. Several pharmacokinetic alterations were observed and this might be caused by the pathological state of type 2 diabetes.
研究领域:
药理学
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分析化学
·
糖尿病研究
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FOOD RESEARCH INTERNATIONAL
·
2026
·
IF 8.8
Yuanyuan Zhao,Yongmao Lu,Tian Yang,Shaohua Hu,Yuanyuan Yan,Xingguo Wang,Wei Wei
Multi-method strategy enhances accuracy in human milk vitamin research. • Mass spectrometry achieved precise 25(OH)D₂/₃ quantification in human milk. • Immunoassays offered rapid screening but showed a 72.98% positive bias. • Liquid chromatography profiled vitamins A and E but lacked sensitivity for D and K. • 25(OH)D₃ increased slightly, while 25(OH)D₂ declined across lactational stages. Accurate analysis of vitamin D in human milk is essential for infant nutrition but remains analytically challenging due to low levels and a complex matrix. This study evaluates a practical multi-method strategy using LC-MS/MS, ELISA, and UPLC-PDA for vitamin D analysis in human milk. LC-MS/MS precisely quantified 25(OH)D₂ and 25(OH)D₃ with assay LOQ of 0.045 ng/mL and 0.100 ng/mL, respectively. ELISA showed a 11.58 ng/mL positive bias of vitamin D which limits use for accurate quantification. UPLC-PDA profiled vitamins A and E effectively but lacked sensitivity for vitamin D. Longitudinally, LC-MS/MS results show 25(OH)D₃ and total 25(OH)D concentrations remained relatively stable, with medians ranging from 0.141 to 0.281 ng/mL and 0.263 to 0.315 ng/mL, respectively, across the study period, while 25(OH)D₂ peaked at 8 weeks before declining. This study establishes LC-MS/MS as the preferred analytical strategy for quantifying 25(OH)D 2 and 25(OH)D 3 in human milk, providing critical data to assess infant nutritional intake and guide clinical interventions. Download: Download high-res image (160KB) Download: Download full-size image
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BULLETIN OF ENVIRONMENTAL CONTAMINATION AND TOXICOLOGY
·
2023
·Vol. 111
·期 4
·1-9
·
IF 2.7
Zheng Handinghong,Wu Qiong,Wu Xiaomao
This study aimed to investigate the dissipation, residues and dietary assessment of kresoxim-methyl in the application of Rosa Roxburghii and soil field using liquid chromatography-tandem mass spectrometry (LC–MS/MS). The results show that kresoxim-methyl in R. roxburghii samples was extracted by acetonitrile and purified by ethyl enediamine-N-propylsilane (PSA), while kresoxim-methyl in soil samples was extracted by acetonitrile and purified by octadecylsilyl solid phase dispersant (C 18 ). 0.1% formic acid (v/v)-water–methanol solution was used as the mobile phase, LC–MS/MS exhibited a good linearity in the range of 0.001–10 mg L −1 . The recoveries of R. roxburghii and soil matrix were 82.48%–102.55%, and the relative standard deviation ( RSD) were 1.13%–4.21%. The limit of detection ( LOD ) and quantification ( LOQ ) of kresoxim-methyl in R. roxburghii and soil samples was 0.50 and 0.60 µg kg −1 , respectively. The dissipation dynamics of kresoxim-methyl in R. roxburghii and soil followed the first-order kinetics, with the half-life of 4.28 and 4.41 days, respectively. The terminal residual amount of kresoxim-methyl in R. roxburghii and soil samples was 0.003–1.764 and 0.007–2.091 mg kg −1 , respectively. The dietary intake risk assessment indicates that a risk quotient ( RQ ) for kresoxim-methyl based on the national estimated daily intake ( NEDI ) of 0.1995 mg was 0.79%, suggesting that the use of kresoxim-methyl on R. roxburghii at recommended dosage was safe to consumers. This study provides the theoretical basis for guiding the rational use of kresoxim-methyl in the production of R. roxburghii .
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JOURNAL OF HAZARDOUS MATERIALS
·
2023
·
IF 13.6
Man-Man Wang,Zi-Ling Li,Han Wu,Ke-Yan Chen,Fan Guo,Gui-Fu Zuo,Yu He,Xue-Bo Yin
Magnetic solid-phase extraction (MSPE) was developed based on a well-designed Fe 3 O 4 -NH 2 @g-C 3 N 4 nanocomposite as sorbent for a mixture of six benzophenones (BPs) in environmental water samples. The composite fabricated via in-situ self-assembled g-C 3 N 4 shell with homogeneous polymerization of cyanuric chloride and cyanuric acid on Fe 3 O 4 -NH 2 core. While high adsorption capacity was derived from g-C 3 N 4 via hydrophobic, π-π and hydrogen bonding interactions to the targets, the fast magnetic separation was realized with Fe 3 O 4 core for less solvent consumption. In combination with LC-MS/MS, the Fe 3 O 4 -NH 2 @g-C 3 N 4 sorbent minimized the interfering components, reduced the matrix effects, and provided the enrichment factors of 121–150 for six BPs with relative standard deviations ≤ 9.7% even after 20 times extraction-desorption cycles. The present method gave the detection limits of 0.3–2.5 ng/L for six BPs with the linear ranges of 1.0–2000 ng/L, and the recoveries of 84.6%−104% in sea water and 86.2%−107% in lake water samples. Thus, the Fe 3 O 4 -NH 2 @g-C 3 N 4 -based MSPE coupled with LC-MS/MS method provided a convenient, efficient, and reliable alternative to monitor trace BPs in environmental water samples.
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Marine Drugs
·
2023
·Vol. 21
·期 10
·502
·
IF 5.4
Yawen Wang,Longjian Zhou,Minqi Chen,Yayue Liu,Yu Yang,Tiantian Lu,Fangfang Ban,Xueqiong Hu,Zhongji Qian,Pengzhi Hong,Yi Zhang
The prevalence of gout and the adverse effects of current synthetic anti-gout drugs call for new natural and effective xanthine oxidase (XOD) inhibitors to target this disease. Based on our previous finding that an edible seaweedPterocladiella capillaceaextract inhibits XOD, XOD-inhibitory and anti-inflammatory activities were used to evaluate the anti-gout potential of differentP. capillaceaextract fractions. Through affinity ultrafiltration coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS), feature-based molecular networking (FBMN), and database mining of multiple natural products, the extract’s bioactive components were traced and annotated. Through molecular docking and ADMET analysis, the possibility and drug-likeness of the annotated XOD inhibitors were predicted. The results showed that fractions F4, F6, F4-2, and F4-3 exhibited strong XOD inhibition activity, among which F4-3 reached an inhibition ratio of 77.96% ± 4.91% to XOD at a concentration of 0.14 mg/mL. In addition, theP. capillaceaextract and fractions also displayed anti-inflammatory activity. Affinity ultrafiltration LC-MS/MS analysis and molecular networking showed that out of the 20 annotated compounds, 8 compounds have been previously directly or indirectly reported from seaweeds, and 4 compounds have been reported to exhibit anti-gout activity. Molecular docking and ADMET showed that six seaweed-derived compounds can dock with the XOD activity pocket and follow the Lipinski drug-like rule. These results support the value of further investigatingP. capillaceaas part of the development of anti-gout drugs or related functional foods.Keywords:Pterocladiella capillacea;xanthine oxidase inhibitors;anti-inflammatory;affinity ultrafiltration LC-MS/MS;molecular networking
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FOOD CHEMISTRY
·
2023
·
IF 8.8
Youzhi Su,Jianjiang Lu,Jun Liu,Fang Li,Ning Wang,Hongqin Lei,Xiaofang Shen
A modified QuEChERS purification–liquid chromatography-tandem mass spectrometry method has been developed to determine 51 pesticide residues with newly established maximum residue limits (MRLs) in foodstuffs. Samples were extracted with acetonitrile under citrate-buffered conditions and purified using a modified QuEChERS method employing hydroxylated MWCNTs , SAX, and C 18 . The limits of quantification ranged from 0.2 to 9.8 µg/kg. Recoveries in ten different foodstuffs ranged from 70.2% to 117.9%, with relative standard deviations between 2.3% and 19.9% at three spiking levels. This method was applied to analyze 352 market samples, detecting 14 pesticides in 97 samples. Notably, Afidopyropen, cyantraniliprole, and fluxapyroxad residues in vegetables exhibited a consistent pattern of higher levels in the spring and winter and lower levels in the summer and autumn. Moreover, the risk assessments for acute and chronic dietary exposure to the 14 detected pesticides indicated that the %ADI and %ARfD were well below 100%.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2019
·
IF 2.813
Zhuowei Shen,Kaifeng He,Mingcheng Xu,Kui Zeng,Jie Pan,Fengting Ou,Jianbiao Yao,Ruwei Wang,Su Zeng
A sensitive and specific bioanalytical method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the quantification of 6-hydroxykynurenic acid (6-HKA) in a small quantity of rat plasma has been developed and comprehensively validated. Tolbutamide (Tol) was used as the internal standard (IS). An aliquot of 50 μL rat plasma sample was deproteinized by 150 μL methanol, and then 100 μL of its supernatant was mixed with 100 μL water after centrifugation . Chromatographic separation was performed on a ZORBAX Eclipse Plus C 18 Rapid Resolution HD column (2.1 mm × 100 mm, 1.8 μm) with a gradient mobile phase consisting of water containing 2 mM ammonium formate and methanol at a flow rate of 0.2 mL/min over a total run time of 5.0 min. The mass spectrometer was operated under multiple reactions monitoring (MRM) mode with the transitions m / z 206.1 → 160.0 for 6-HKA and m/z 269.0 → 170.0 for Tol. The linear range was 2.5–250 ng/mL with the square regression coefficient (r 2 ) of 0.997. The lower limit of quantification (LLOQ) was 2.5 ng/mL (Relative Error, RE +1.6% and RSD 4.8%, n = 5). The intra- and inter-day precision and accuracy was <13.3%. The mean recovery of 6-HKA in rat plasma was between the range of 99.3–103.4%. This method was successfully applied to study the pharmacokinetics of 6-HKA in rats after oral administration at a single dose of 20.0 mg/kg and after tail intravenous injection at a single dose of 2.0 mg/kg. Pharmacokinetic parameters bioavailability, C max, oral , T max, oral , AUC 0–24h, oral , AUC 0–∞, oral , AUC 0–24h, iv and AUC 0–∞, iv were 3.96%, 152.0 ± 85.5 ng/mL, 0.4 ± 0.1 h, 340.0 ± 136.3 ng/mL ∗ h, 369.5 ± 135.0 ng/mL ∗ h, 906.6 ± 324.1 ng/mL*h and 932.9 ± 336.5 ng/mL ∗ h, respectively.
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BIOMEDICAL CHROMATOGRAPHY
·
2017
·Vol. 32
·期 3
·e4126
·
IF 1.613
Fuguo Shi,Hong Pan,Yi Li,Linyan Huang,Qin Wu,Yuanfu Lu
Genipin (GP), an active metabolite of geniposide (GE), exhibits more potent pharmacological effects than its parent compound. In this paper, a sensitive LC-MS/MS method was developed and fully validated for the simultaneous determination of GE and GP in rat plasma. We found that GP degraded rapidly in rat plasma at room temperature as a result of irreversible binding with the endogenous nucleophiles in plasma. GP was stable when the sample's pH was ≤4.0. The degradation of GP in rat plasma was well prevented by immediate addition of 5% glacial acetic acid to the freshly collected plasma. The detection was performed on a tandem mass spectrometer coupled with electrospray ionization source in negative mode. Quantification was conducted by multiple reaction monitoring of the transitions [M + CH 3 COO] − m/z 447.3 → 225.3 for GE and [M − H] − m/z 225.2 → 123.1 for GP. The method exhibited high sensitivity (LLOQ 1 ng/mL for GE and 0.2 ng/mL for GP) by selecting the acetate adduct ions as the precursor ions for GE. The robust developed method was successfully applied to a pharmacokinetic study in rats after oral administration of GE.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2025
·
IF 2.8
Bohan Liang,Yanjie Li,Lingmei Xu,Li Wang,Quankun Zhuang,Shiqi Dong,Huirong Fan
XZP-3287(bireociclib) is a novel and selective inhibitor of the cell cyclin-dependent kinases 4/6 (CDK4/6), which is primarily employed for the treatment of breast cancer in clinical trials . In this study, a novel and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the simultaneous determination of XZP-3287 and its metabolites XZP-5286, XZP-3584 and XZP-5736 in human plasma in accordance with international conference on harmonization of technical requirements for registration of Pharmaceuticals for Human use (ICH) guideline R3 (M10) guideline. The multiple reaction monitoring mode (MRM) of mass spectrometer was used and all compounds were monitored in electrospray ionization (ESI+) mode. The correlation coefficients (R 2 ) of all calibration curves for linear regression were greater than 0.99. The intra- and inter-day precision of XZP-3287 and its metabolites XZP-5286, XZP-3584 and XZP-5736 were determined to be 5.2 %–5.5 %, 14.9 %–10.1 %, 6.9 %–13.8 % and 7.3 %–5.6 %, and their accuracy were determined to be 5.2 %–6.0 % 6.9 %–4.4 %, 11.1 %–5.0 % and 7.4 %–5.6 %, respectively. In conclusion, a method for the simultaneous detection of the pharmacokinetic profiles of XZP-3287 and its metabolites in human plasma had been successfully developed. The results demonstrated the efficacy, sensitivity, and reliability of this method
研究领域:
药物分析
·
临床药理学
·
肿瘤学
·
质谱分析
·
药物代谢
·
生物分析化学
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危险品化学品经营许可证（带存储）