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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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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ACS Omega
·
2025
·
IF 4.3
Tingting Lou,Benkai Qin,Jiaqi He,Hongliu Qu,Haiyan Rong,Qunan Cheng,Weiyong Lu,Yaqin Liu,Yonghua Yu
A rapid, specific, and sensitive LC–MS/MS method for the determination of sulindac and its metabolite Su-EP-C in human EDTA-K2 plasma was developed. The method was fully validated using sulindac-d3 and Su-EP-C-d3 as internal standards. Separation was performed on a Kinetex C18 analytical column (100 Å, 50 × 2.1 mm, 5 μm). MPA consisted of 0.05% formic acid (FA) in water, while MPB comprised 0.05% FA in ACN. The flow rate was maintained at 0.300 mL/min, and the injection volume was 3 μL. Mass spectrometry conditions: ESI, positive mode, MRM. The linear range of detection was from 60.00 to 24,000.00 ng/mL for sulindac and from 30.00 to 12,000.00 ng/mL for Su-EP-C. The intra- and interbatch accuracy deviations of sulindac ranged from −5.1 to 5.0%, and the intra- and interbatch precision ranged from 3.3 to 4.2%. The intra- and interbatch accuracy of Su-EP-C ranged from −3.9 to 6.9%, and the intra- and interbatch precision ranged from 4.8 to 7.2% at all concentration levels. At a dilution of 10, the deviation for sulindac was 3.5% and the precision was 1.5%; the deviation for Su-EP-C was 2.7%, and the precision was 4.4%. The plasma matrix, at both −20 °C and −70 °C, remained stable for 52 days with 5 freeze–thaw cycles. The method was successfully applied to fasting and postprandial pharmacokinetic clinical trials of orally administered sulindac tablets.
研究领域:
药物分析
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临床药理学
·
生物分析化学
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质谱分析
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药代动力学
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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
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临床药理学
·
肿瘤学
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质谱分析
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药物代谢
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生物分析化学
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JOURNAL OF MASS SPECTROMETRY
·
2026
·Vol. 61
·期 8
·e70088
·
IF 2.1
Liping Yang,Bingling Gao,Tao Yang,Liping Tang,Ying Kan,Keqi Sun,Peng Xiao
Dehydroepiandrosterone sulfate (DHEAS), a crucial steroid hormone for adrenal function and pubertal development, is highly associated with related diseases. This study aims to develop and validate an isotope dilution liquid chromatography tandem mass spectrometry (ID-LC–MS/MS)-based candidate reference measurement procedure (cRMP) for quantifying serum DHEAS. Serum samples were prepared by protein precipitation with acetonitrile and separated on a reversed phase column. Assay validation was conducted under the guidance of standard documents, including C62-A, EP6-A, EP10-A3, and C50-P endorsed by the Clinical and Laboratory Standards Institute (CLSI). The cRMP was established and proven to be highly specific without significant matrix effect and able to accurately quantify DHEAS in human serum. The intra-assay and inter-assay imprecision ranged from < 0.1 to 1.0% and from 1.0 to 1.1%, respectively. Trueness was assessed by recovery rate from 99.6 to 101.2%. The limit of detection (LoD) was 0.270 nmol/L, and the lower limit of the measuring interval (LLMI) was 12.1 nmol/L. A linear correlation ranged from 7.60 to 41 858 nmol/L was observed with a correlation coefficient > 0.999. R 2 value of linear regression analysis between this method and clinical immunoassays was ≥ 0.990. The relative expanded uncertainty was 1.5%–2.5% over the concentration range of 12.1–33 043 nmol/L. This study developed an ID-LC–MS/MS-based cRMP, which provided high specificity, trueness, and precision for serum DHEAS quantification, contributing to the DHEAS measurement standardization and traceability.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2026
·
IF 4.1
Guan Xinhui,Zhang Yuying,Ma Xiaoqiao,Wang Haiyan,Qiao Xiaoqiang,Gu Xiaofei
Comprehensive characterization of exosomal phospholipids is essential for understanding cancer-associated metabolic alterations and discovering potential biomarkers, but remains challenging due to their extensive structural diversity and the limited selectivity and coverage of conventional liquid chromatography-tandem mass spectrometry (LC-MS/MS) approaches. In this study, an ionic liquid-functionalized styrene-maleic anhydride copolymer brush stationary phase (Sil-BHHICl) was developed and integrated into an offline two-dimensional (2D) LC-MS/MS platform for comprehensive exosomal phospholipid profiling. The Sil-BHHICl stationary phase exhibited a hydrophilic interaction/reversed-phase mixed-mode retention mechanism and provided enhanced selectivity toward phospholipids, enabling efficient separation at both the phospholipid-class and molecular-species levels. The developed analytical platform enabled comprehensive profiling of plasma-derived exosomal phospholipids, resulting in the identification of 274 molecular species belonging to 10 phospholipid classes. Lipidomic analysis of plasma exosomes from breast cancer patients and healthy controls revealed distinct phospholipid alterations associated with breast cancer and identified five candidate biomarkers, among which LysoPC-O (16:0) exhibited the strongest discriminatory ability. Pathway enrichment analysis further indicated that the altered phospholipids were predominantly associated with glycerophospholipid metabolism, suggesting extensive lipid metabolic remodeling in breast cancer. Overall, this study establishes a mixed-mode chromatographic platform for high-coverage exosomal phospholipid profiling and demonstrates its potential for lipidomics-based biomarker discovery and investigation of disease-associated metabolic alterations. Graphical abstract
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CLINICA CHIMICA ACTA
·
2026
·
IF 4.1
Xin-Yu Wu,Xiao-Kang Fu,Ao Li,Wei Zhang,Han-Peng Jiang,Na An,Quan-Fei Zhu,Shao-Ting Wang,Yu-Qi Feng
Background Therapeutic drug monitoring (TDM) of tacrolimus requires accurate, high-throughput methods, but conventional liquid chromatography–tandem mass spectrometry (LC-MS/MS) is limited by lengthy run times and complex sample preparation. Methods We developed a chromatography-free assay for quantification of tacrolimus in whole blood by integrating cold-induced phase separation with acoustic ejection mass spectrometry (AEMS). This workflow only requires less than 10 μL of whole blood, eliminates centrifugation, and enables direct nanoliter-scale injection into the mass spectrometer. The AEMS assay performance was validated in accordance with CLSI C62-A and ICH M10 guidelines using 62 patient samples and matrix-matched calibrators, demonstrating its suitability for high-throughput therapeutic drug monitoring. Results The AEMS assay exhibited excellent linearity (0.5–50 μg/L; R 2 = 0.9987), with a lower limit of quantification of 0.5 μg/L, which was well below clinically relevant trough concentrations. Accuracy (93.3%–100.1%) and precision (intra-day RSD: 3.7%–11.3%; inter-day RSD: 2.3%–12.4%) met regulatory acceptance criteria. Results showed strong concordance with routine LC-MS/MS (Spearman ρ = 0.972; Passing–Bablok slope = 1.100 [95% CI: 1.026–1.177]). The total analysis cycle time was less than 3 s per sample, enabling a throughput exceeding 1000 samples per hour theoretically. Conclusion This study establishes the first chromatography-free mass spectrometry platform validated for clinical TDM of TAC. By integrating ultra-high throughput capability, minimal sample consumption, and robust analytical performance, the AEMS workflow offers a transformative analytical solution for high-demand clinical environments, including transplant centers and pediatric monitoring settings.
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JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2025
·Vol. 63
·期 10
·
IF 1.3
Zheng Jun-tao,Kong Jia-he,Yang Ting,Wang Xue-ding,Guan Shao-xing,Guan Yan-ping,Huang Min,Gao Xiang,Chao Kang,Zhu Xia
Deoxythioguanosine (dTG), incorporated into DNA as DNA-TG, is considered a more relevant thiopurine metabolite than erythrocyte thioguanine nucleotides, as erythrocytes are not the drug target. We established a simple and sensitive liquid chromatography–tandem mass spectrometry method to detect dTG in human blood nucleated cell DNA and validated its clinical applicability in Chinese patients with inflammatory bowel disease to improve individualized thiopurine treatment. dTG was released from 1 μg DNA in a single hydrolysis step, separated by the X-Terra RP18 column and quantified by tandem mass spectrometry with 2′- Deoxyguanosine-13C,15N2 as the internal standard. The calibration curve covered eight concentration levels (0.125–25 ng/mL) with the correlation coefficients r2 ≥ 0.99. The intra- and inter-assay variability was achieved less than 9.9%. This method was employed in a study where a total of 125 inflammatory bowel disease patients with a median DNA-TG level of 279.7 fmol/μg DNA (interquartile range 183.5 ~ 410.6 fmol/μg DNA). Nucleoside diphosphate-linked moiety X-type motif 15 variant carriers (*2, *3, *5, *6) showed significantly higher DNA-TG/dose and DNA-TG/erythrocyte thioguanine nucleotides ratios than wild-type patients (P = 0.0023, P = 0.0001). In summary, this method was simple and stable to detect dTG in DNA, which may act as a promising biomarker predicting the toxicity and efficacy in patients treated with thiopurine.
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MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Lingcan Kong,Haixin Chen,Qiaoyan Liu
Excessive intake bioamines is harmful to human health, and thus the development of simple, rapid and efficient detection method of bioamines in food is urgent. Herein, an unprecedented method based on a commercial molecular sieve has been developed for the determination of four bioamines (cadaverine, tyramine, histamine and tryptamine) in fruit wines by dispersive solid phase microextraction (D-μSPE) coupled to liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS). The extraction process of ultra-stable Y-type molecular sieve (USY) on bioamines belongs to physisorption, and the adsorption pattern is found in good accord with the Langmuir isotherm model. Theoretical and experimental analyses are further used to explore their binding energies, binding constants, and the maximum adsorption capacity. It is found that the adsorption is driven mainly by hydrogen bonds between USY and bioamines and water molecules. Moreover, the extraction efficiency is dependent on the binding constants and the maximum adsorption capacity of USY. The optimization of adsorption-desorption process involves the USY amount, extraction time, desorption solvent, desorption time, desorption number and cyclic usage number of USY. Under the optimum conditions, the limits of detection and quantification were found in the range of 0.2–2.5 μg L −1 and 0.6–8 μg L −1 with intra-day and inter-day precision and recoveries in a fruit wine in the range of 1.3 %–7.9 % and 91 %–104 %, respectively. Owing to the efficient enrichment and edulcoration functions of USY, the method shows negligible matrix effect and is simple, rapid, and has the potential to apply in routine work.
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CLINICAL BIOCHEMISTRY
·
2025
·
IF 2.1
Chunyan Zhang,Nan Bai,Yanling Yang,Yuxuan Cheng,Xiyu He,Meng Wang,Honghui Zhou,Yaping Tian
Objectives Metabolic disorders in newborns can cause significant morbidity and mortality if not diagnosed and managed early. In this study, we developed and validated a reliable LC-MS/MS method to simultaneously quantify methylmalonic acid, methylcitric acid, malonic acid, ethylmalonic acid, and total homocysteine associated with metabolic disorders. Design and methods According to Clinical Laboratory Standards Institute (CLSI) guidelines, various analytical performances (i.e., precision, linearity, accuracy and reference intervals) were rigorously evaluated. Meanwhile, sample preparation, chromatographic separation and mass spectrometric detection and incorporating stable isotope-labeled internal standards were optimized. Furthermore, calibrators and quality controls were developed to ensure standardization and traceability. Results The coefficient of variations for precision were less than 10.0 %. Meanwhile, the results showed high accuracy (recoveries: 94.57 %–109.60 %) and robust linearity (R 2 > 0.9935) over clinically relevant ranges. The limits of detection and limits of quantification for all analytes were established, enabling sensitive detection of pathological elevations. Reference intervals for pediatric populations (ages 0–1 month and 2 months to 18 years) were determined, providing essential baselines for clinical interpretation. Conclusions The newly developed method demonstrated good analytical performance and offers a standardized, high-throughput solution for clinical laboratories to improve early diagnosis and personalized management of metabolic diseases.
研究领域:
临床化学
·
代谢组学
·
新生儿筛查
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质谱分析
·
生物医学检验
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危险品化学品经营许可证（带存储）