JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2026
·
IF 2.5
Chang Wang,Shijiao Zhang,Wenqing Liu,Zizhuo Shao,Aijia Cao,Chen Jia,Xia Song,Haisheng Jiao,Yinliang Bai
A rapid UPLC-MS/MS method for bupivacaine TDM was developed and validated (run time 2.5 min). • The assay meets FDA/Chinese Pharmacopoeia criteria with LLOQ of 1.0 μg/L using only 50 μL plasma. • Simple protein precipitation ensures high recovery (> 90%) and negligible matrix effects. • Clozapine is introduced as a cost-effective internal standard with excellent reproducibility. • Clinical application in 40 patients revealed distinct PK profiles of conventional vs. liposomal bupivacaine. Background Bupivacaine (BPC) is a cornerstone of perioperative analgesia, yet its narrow therapeutic index and high interindividual pharmacokinetic variability complicate dosing and increase toxicity risks. A robust, high-throughput analytical platform is needed to support therapeutic drug monitoring (TDM) and individualized therapy. Methods A rapid ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for quantifying BPC in human plasma was developed and fully validated according to FDA and Chinese Pharmacopoeia guidelines. Sample preparation consisted of a simple protein precipitation step using acetonitrile containing clozapine as the internal standard. Chromatographic separation was achieved within 2.5 min on a C18 column using gradient elution, enabling high-throughput analysis suitable for routine TDM. Results The method demonstrated excellent linearity from 1.0 to 500.0 μg/L ( R 2 > 0.995) and a short run time of 2.5 min, allowing batch analysis of up to 50 samples within 3 h. Intra- and inter-day precision (coefficient of variation) were < 15%, and accuracy ranged between 85% and 115% across quality control levels. The lower limit of quantification was 1.0 μg/L. Extraction recovery was consistent (90.9%–94.5%) and matrix effects were negligible. In a pilot clinical study involving 40 patients, the method successfully differentiated the pharmacokinetic profiles of two formulations: conventional BPC (75 mg) showed rapid distribution and elimination, while liposomal BPC (133 mg) maintained sustained plasma concentrations over 24 h. Conclusion This validated UPLC-MS/MS method is a rapid, sensitive, and high-throughput tool for BPC TDM that represents a promising candidate for implementation in clinical laboratories following appropriate local validation. Its successful clinical application highlights its utility in characterizing formulation-dependent pharmacokinetics and could assist in the development of precision dosing in perioperative analgesia to optimize efficacy and safety.
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FOOD HYDROCOLLOIDS
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2025
·
IF 12.4
Yanyun Zhu,Yafei Dong,Dandan Li,Bingge Liu,Qing Ye,Kouadio Jean Eric-Parfait Kouame,Ebenezer O. Falade,Sami Ullah,Ishtiaq Ahmad,Xingqian Ye
Glycosidic linkage analysis is crucial for elucidating the structure-activity relationships of polysaccharides, but existing GC-MS methods have limitations in practical applications. This study developed a simple, efficient, and sensitive UPLC-QqQ-MS/MS method for glycosidic linkage analysis, validated using glucose-based oligosaccharides and polysaccharides. 16 glucose glycosidic linkage standards were synthesized using anion reconstruction, partial methylation, and PMP derivatization. Samples underwent permethylation and PMP derivatization before UPLC-QqQ-MS/MS analysis. The accuracy and feasibility of the method were validated by comparing the results with the synthesized glycosidic linkage standards and known glycosidic linkage information. Results showed that the LC-MS-MRM spectra of the 1-4-Glc glycosidic linkages in lactose, maltose, and cellulose exhibited identical retention times and characteristic fragment ions, consistent with the synthesized 1-4-Glc standard. This confirmed the accuracy of the synthesized standards and the feasibility of the LC-MS method for detecting glycosidic linkages. Similarly, the retention times and characteristic fragment ions of the T-Glc linkages in maltose and Aspergillus Niger disaccharide, the 1-3-Glc linkage in Aspergillus Niger disaccharide, and the 1-6-Glc linkages in glucan were consistent with their corresponding standards. These results demonstrate that the UPLC-QqQ-MS/MS method can be used for qualitative and quantitative analysis of both unknown and known glycosidic linkages in oligosaccharides and polysaccharides.
研究领域:
分析化学
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碳水化合物化学
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结构生物学
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质谱分析
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2024
·
IF 2.8
Yuyu Cao,Dayi Xu,Liping Zhang,Kaiyuan Pang,Liyuan Zhang,Xiaobao Wei,Zengxian Sun
The study introduces a robust analytical method based on UPLC-MS/MS for quantifying thiol amino acids, including cysteine (Cys), cysteinylglycine (CG), homocysteine (Hcy), and glutathione (GSH), in their total and total free forms within human plasma. An optimized blank matrix was employed for accurate quantification of endogenous compounds. The method exhibited excellent linearity, precision, accuracy, recovery, and stability, making it highly suitable for plasma analysis. Distinct differences in plasma levels of GSH, Cys, Hcy, and CG across various forms (total, total free, native prototype, and symmetrical oxidation) were observed between healthy individuals and chronic kidney disease (CKD) patients. Comprehensive correlation and receiver operating characteristic (ROC) analyses revealed disrupted thiol amino acid metabolism in CKD, accompanied by heightened oxidative stress. Notably, various forms of Cys and Hcy correlated significantly with renal function markers and demonstrated high diagnostic efficacy in ROC evaluation, with Cys, particularly Cys (F), outperforming others. Hcy further complements Cys in assessing renal function impairment severity.
研究领域:
临床医学
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代谢组学
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肾脏病学
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JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Chunyi Yu,Xujing Kong,Wenting Li,Boyu Li,Baorong Chen,Mengyao Gao,Susu Cai,Yun Wei
Steroid hormones constitute a group of hormones with molecular weights ranging from 200 to 400 daltons, characterized by their highly similar chemical structures. Each hormone within this group holds significant value for the diagnosis of various diseases. Accurate clinical measurement of the levels of each hormone is crucial for the diagnosis in clinical settings. Due to the wide variety and different properties of steroid hormones in organisms, sample pretreatment is the rate-limiting step for analysis and detection. In this paper, a magnetic molecule-imprinting polymer (MMIPs) was prepared by surface imprinting on silicon coated magnetic spheres, and a detection method of MMIPs-combined with liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for 19 steroid hormones in plasma was developed and verified. Fourier transform infrared spectroscopy, field emission scanning electron microscopy and transmission electron microscopy were used to confirm the formation of MMIPs materials, and the conditions of material synthesis and pretreatment of steroid hormones from plasma were optimized. The detection method was evaluated by using linearity, LOD and LOQ, precision, accuracy and matrix effect. The linearity of 19 steroid hormones was good, and the linear correlation coefficient was greater than 0.995. The coefficients of variation were 2.1-9.8% and 1.1-9.7% for intra-day and inter-day, respectively, and the recoveries were 83.6%-118.2% at low concentration, and the recoveries of medium and high concentrations were 94.6%-113.8% and 89.5%-113.6%, respectively. The coefficient of variation of Relative matrix effect of 19 steroid hormones measured in different batches of plasma was 2.1-5.4% after isotope internal standard correction, which eliminated the influence of matrix effect.
研究领域:
分析化学
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医学检验
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生物化学
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JOURNAL OF ENVIRONMENTAL SCIENCE AND HEALTH PART B-PESTICIDES FOOD CONTAMINANTS AND AGRICULTURAL WASTES
·
2026
·
IF 2
Ning Li,Yunyu Tang,Wenwen Zhang,Yang Bai,Fengshou Sun,Jin Lin
The combined application of difenoconazole and pyraclostrobin is a common strategy to combat early blight in potatoes; however, a comprehensive understanding of their co-residue behavior and associated dietary risks remains limited. In this study, a modified QuEChERS method coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed and validated for the simultaneous determination of difenoconazole and pyraclostrobin residues in potatoes. The calibration curves showed excellent linearity over the concentration range of 0.002–0.2 mg/L. At fortification levels of 0.02, 0.2, and 2 mg/kg, the average recoveries of difenoconazole ranged from 94.8 to 100.4%, with relative standard deviations (RSDs) of 0.56–1.81%; the average recoveries of pyraclostrobin ranged from 95.2 to 99.8%, with RSDs of 0.97–1.62%. The limit of quantification (LOQ) of both compounds was 0.02 mg/kg, and the instrumental limit of detection (LOD) was 2.00 × 10 g. This sensitivity is substantially better than that of conventional HPLC-UV methods (which typically exhibit LODs around 10−9 g), and the LOQ aligns with the maximum residue limit (MRL) of 0.02 mg/kg established in China. Dietary risk assessment indicated that the risk quotients (RQs) were 0.993 and 0.956 for difenoconazole and pyraclostrobin, respectively, demonstrating that the health risks to consumers are acceptable.
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MOLECULES
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2022
·Vol. 27
·期 13
·4129
·
IF 4.927
Taiyu Wang,Hailong Yang,Jie Yang,Ningjie Guo,Guodong Wu,Xueyu Xu,Ming An
A novel method of ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed for the identification and quantification of four potential genotoxic impurities (PGIs) in the active pharmaceutical ingredients of TSD-1, a novel P2Y12receptor antagonist. Four PGIs were named, 4-nitrobenzenesulfonic acid, methyl 4-nitrobenzenesulfonate, ethyl 4-nitrobenzenesulfonate, and isopropyl 4-nitrobenzenesulfonate. Following the International Conference of Harmonization (ICH) guidelines, this methodology is capable of quantifying four PGIs at 15.0 ppm in samples of 0.5 mg/mL concentration. This validated approach presented very low limits (0.1512–0.3897 ng/mL), excellent linearity (coefficients > 0.9900), and a satisfactory recovery range (94.9–115.5%). The method was sufficient in terms of sensitivity, linearity, precision, accuracy, selectivity, and robustness and, thus, has high practicality in the pharmaceutical quality control of TSD-1.Keywords:UPLC-MS/MS;genotoxic impurities;TSD-1;active pharmaceutical ingredients;quantitation;method validation
研究领域:
药物分析
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制药工程
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分析化学
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MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 8
·2861-2870
·
IF 4.58
Qian Liangliang,Li Xiaoqing,Qi Feifei,Li Jian,Lu Lingeng,Xu Qian
An amino-functionalized grooved polyacrylonitrile nanofiber mat was modified by both functional groups and in terms of surface morphology. The mat is shown to represent a viable adsorbent for solid-phase extraction of six priority phenolic pollutants and three phenolic xenoestrogens (phenol, 3-methoxyphenol, 4-nitrophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol, pentachlorophenol, 4-tert-octylphenol, 4-nonylphenol and bisphenol A) from environmental water samples. Under optimized conditions, the analytes were completely extracted from 90 mL of water sample by using only 9 mg of the mat material. Following elution with an ammoniacal methanol-acetone mixture, the eluent was directly submitted to UPLC-MS/MS or HPLC with DAD detection. Satisfied linearity in range of 50 pg·mL −1 to 100 ng·mL −1 was achieved. The detection limits ranged from 4 to 60 pg·mL −1 which revealed the excellent sensitivity of the method in comparison to standardized and other techniques. The recoveries ranged from 82.4% to 111.4%, with the relative standard deviations of 4.0% to 11.4% (for n = 6). The method was applied to the determination of nine phenolic pollutants in water samples collected from sixteen inflow rivers and six Taihu Lake regions.
Amino-functionalized grooved nanofibers mat-based solid-phase extraction for simultaneous determination of nine phenolic pollutants in environmental water
研究领域:
环境科学
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分析化学
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纳米技术
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水处理
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FITOTERAPIA
·
2023
·
IF 3.4
Nan Zhang,Junwei Zhang,Weiqi Cui,Deqiao Wu,Jingxian Zhang,Bo Wei,Lingbo Qu,Xia Xu
Artemisia argyi H.Lév. & Vaniot, a traditional Chinese medicine with a history spanning over two millennia, has been extensively used in folk medicine to treat dysmenorrhea, uterine bleeding and inflammation. Recent studies have demonstrated that the essential oil extracted from Artemisia argyi H.Lév. & Vaniot, known as AAEO, exhibits significant anti-tumor properties against liver and lung cancers. There is a scarcity of research on the potential impact of AAEO on pancreatic cancer (PC) cells. In this study, UPLC-MS/MS-based metabolomics method was established to evaluate the effect of AAEO on the proliferation of PC cells. The differential compounds included 5-oxoproline, glutamate, γ-glutamylcysteine, glutathione, arachidonic acid, adrenal acid and linoleic acid were detected by metabolomics, enriching in the γ-glutamyl cycle and polyunsaturated fatty acid metabolism, which were closely related to ferroptosis. Meanwhile, AAEO dramatically increased the levels of intracellular iron ion via up-regulation of TFR1, augmented reactive oxygen species and malondialdehyde in a dose-dependent manner by down-regulation of γ-glutamyl cycle through decreasing expressions of SLC7A11. Additionally, β-caryophyllene oxide, one of the main components of AAEO, could covalently bind to Cys in SW1990 cells to form a conjugate Cpo-Cys, resulting in the inhibition of glutathione synthesis. Importantly, the ferroptosis inhibitor deferoxamine significantly blocked the inhibitory effect of AAEO on SW1990 cells. Meanwhile, β-caryophyllene oxide, dihydro-β-ionone and α-bisabolol had strong binding force with GPX4, SLC7A11 and TFR1, respectively. These findings showed that AAEO induced ferroptosis via regulation of γ-glutamyl cycle by SLC7A11 and iron disorders by TFR1. Our study discovered AAEO as a potential therapeutic approach to induce ferroptosis to prevent or treat PC.
研究领域:
肿瘤学
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药理学
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代谢组学
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中医药
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高影响因子
MICROCHIMICA ACTA
·
2025
·Vol. 192
·期 11
·1-18
·
IF 5.3
Xie Kexin,Wang Chunfeng,Pang Ningjia,Cheng Yanan,Chen Mengyi,Mu Taotao,Xiao Deli,Di Bin
The design and synthesis of Fe 3 O 4 @PDA@poly(AA-co-EGDMA) nanoparticles (NPs) as a novel magnetic solid-phase extraction (MSPE) material for efficient enrichment and detection of synthetic cannabinoids (SCs) of various structures in large-volume wastewater is reported. The Fe 3 O 4 @PDA@poly(AA-co-EGDMA) NPs were synthesized via a two-step process involving dopamine polymerization and functionalization with poly(acrylic acid-co-ethylene glycol dimethacrylate) polymers, providing hydrophobic and acidic functional groups for enhanced analyte adsorption. An MSPE-ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and optimized for the detection of 24 SCs in wastewater. The method exhibited excellent analytical performance with good linearity ( R > 0.99), low limits of quantification (LOQ, 0.02–0.1 ng/L), and good precision with recoveries ranging from 50.20 to 92.72%. The method is capable of reliably analyzing trace SCs in large volume samples (300 mL and 1 L). This study introduces a simple, rapid, and cost-effective MSPE-UPLC-MS/MS approach for detecting SCs in complex environmental samples. The proposed method offers significant potential for wastewater-based epidemiology (WBE) applications, providing a valuable tool for monitoring drug use trends, public health surveillance, and regulatory enforcement. Graphical
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ACS Omega
·
2026
·
IF 5.2
Liwei Zhao,Jianlong Ma,Fengxia Hao,Xuebin Li,Qingqi Feng
As a traditional Chinese medicine, bitter almonds contain amygdalin, which can be hydrolyzed by β-glucosidase to release highly toxic hydrogen cyanide. There are safety hazards in clinical use, and high-temperature pretreatment is required for use. This study is based on the differences in β-GC activity of bitter almonds treated with different pretreatment methods. SPME-GC-MS and UPLC-MS/MS combined techniques were used to analyze the metabolic profile differences before and after processing from both volatile and nonvolatile dimensions. A total of 30 compounds were identified through volatile component analysis, among which terpenoids such as d-limonene and linalool were significantly upregulated during steaming, while benzyl alcohol was significantly downregulated. A total of 199 metabolites were identified through nonvolatile component analysis, and 80 significantly different metabolites were screened. Among them, the number of downregulated substances in steaming (45) far exceeded that in boiling (19) and frying (23), showing a clear trend of substance degradation. Of particular importance is the significant degradation of the cyanide alkaloid prunasin during the processing, resulting in the formation of volatile products such as benzaldehyde and hydrogen cyanide, which confirms the detoxification mechanism of processing at the molecular level. KEGG pathway enrichment analysis revealed that differential metabolites mainly involve 56 pathways such as α linolenic acid metabolism and purine metabolism, constructing a complex metabolic network during the processing.
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FOOD CHEMISTRY
·
2026
·
IF 10.4
Rong Bao,Rongting Zhuo,Zhuxiang Zhong,Yan Yang
Antibiotic residues in animal-derived foods raise food safety concerns. This study developed a QuEChERS–UPLC–MS/MS method for the simultaneous detection of multiple antibiotics in animal-derived foods. Key QuEChERS pretreatment parameters were systematically optimized using response surface methodology with a central composite design to identify the optimal extraction solvents, salting-out agents, and clean-up sorbents. Method validation met the requirements of European Commission Implementing Regulation (EU) 2021/808, confirming suitability for rapid determination of 85 antibiotics across diverse food matrices. Analysis of 590 samples detected antibiotic residues in 39.8% of samples, representing 36 different antibiotics. Health risk assessment showed a Hazard Index (HI) < 1, indicating low risk at current consumption levels for the local population. Nevertheless, this high detection frequency highlights the need for continued monitoring of antibiotic residues in animal-derived foods.
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JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Simin Xu,Wenxia Zheng,You Zeng,Xingguo Tian,Xiaoyan Xu
As a local pig breed, Mi pig (MP) is highly prized by Chinese consumers for its unique flavor and exceptional quality. This study aimed to investigate the differences in volatile profile between MP and commercial crossbred pigs (CP), as well as potential factors contributing to these variations. Results showed that MP had significantly higher intramuscular fat (IMF) content (7.75 %) and unsaturated fatty acid (UFA) content (56.44 %) compared to CP. Utilizing headspace solid-phase microextraction-gas chromatography tandem mass spectrometry (HS-SPME-GC–MS) and lipidomics, 14 volatile compounds and 310 lipids were identified as key factors influencing the flavor differences between the two breeds. Specifically, UFAs produced through glycerophospholipid and glycerolipid metabolic pathways play an essential role in developing the rich MP flavor. Our findings provide valuable insights into the underlying mechanisms responsible for the distinctive flavor of MP, highlighting the role of lipid metabolism in flavor formation.
研究领域:
食品科学
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动物科学
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高影响因子
危险品化学品经营许可证（带存储）