ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2024
·
IF 3.8
Yan Qiaofang,Huang Fei,Wang Chuyang,Zhan Min,Zhang Qiaoxuan,Huang Di,Yan Jun,Lin Haibiao,Huang Xianzhang,Han Liqiao
Digoxin, a cardiac glycoside, is widely used in the treatment of cardiovascular diseases. Due to its narrow therapeutic range, precise monitoring of its blood concentration is essential. A reference measurement procedure (RMP) is pivotal for ensuring result accuracy and comparability. The RMP for serum digoxin by ID-LC-MS/MS was optimized with sample pre-treatment and detection processes, and the bracketing calibration method was used, which facilitates more accurate measurement, especially for extreme concentrations. The performance of this optimized RMP was thoroughly evaluated. The limit of detection (LoD) was 0.05 ng/mL (0.06 nmol/L) and the lowest limit of quantification (LLoQ) was 0.10 ng/mL (0.13 nmol/L). The intra- and inter-assay imprecisions were 2.24%, 2.51%, 1.40% and 1.72%, 1.65%, 0.97% at 0.5, 2.0, 5.0 ng/mL, respectively. Recoveries were 99.63 to 101.42% and the linear response ranged from 0.1 to 10.0 ng/mL. The relative bias was 0.41% and 2.00% of our results compared with the median of all participating reference laboratories for IFCC-RELA (External Quality Assessment Scheme for Reference Laboratories in Laboratory Medicine) 2023A and 2023B. The uncertainty, calibration and measurement capability (CMC) of this method were also evaluated. The optimized RMP was applied in the Trueness Verification Plan of Southern China, which indicates significant differences among clinical systems, highlighting the need for standardization efforts. In addition, two commonly used clinical systems which employed immunoassay methods were compared with this optimized RMP, and 26 individual serum samples were analyzed. The good correlations indicate the feasibility of standardization for serum digoxin. The optimized RMP serves as an accurate reference baseline for routine methods, aiming to enhance the accuracy and precision of measurements in clinical laboratories. Graphical Abstract
研究领域:
临床化学
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药理学
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分析化学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
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2021
·
IF 7.514
Renyong Liao,Qiang Xia,Changyu Zhou,Fang Geng,Ying Wang,Yangying Sun,Jun He,Daodong Pan,Jinxuan Cao
The spoiled dry-cured ham commonly shows unpleasant taste and odour. To deepen the understanding in the formation mechanism of unpleasant taste in spoiled ham, sensory attributes, texture parameters, protein degradation, metabolites were investigated between normal and spoiled hams; the relationship between the sensory quality and metabolites of dry-cured ham was further evaluated by partial least square discriminant analysis (PLS-DA). The scores of richness and overall acceptance were significantly lower in spoiled ham, and more than 12.5-fold values in adhesiveness were found in spoiled ham than normal ham. Myofibrillar proteins including actin, troponin-T and myosin light chain showed excessive degradation in spoiled ham. Forty-two kinds of metabolites mainly derived from protein degradation were identified by LC-MS/MS, and amino acid derivatives and oligopeptides were the key components to distinguish spoiled and normal hams demonstrated by PLS-DA. Purine metabolism, pyrimidine metabolism and protein degradation were the main metabolism pathways in spoiled ham.
研究领域:
食品科学
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分析化学
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代谢组学
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感官科学
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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
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2018
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IF 2.746
Guihua Gao,Yanyan Xing,Tingting Liu,Jian Wang,Xiaohong Hou
Four water stable metal-organic frameworks (MOFs), MIL-101(Cr), MIL-100(Fe), MIL-53(Al), and UiO-66(Zr), were used as adsorbents for concentration of four androgens and progestogens from water. The adsorption abilities of target analytes on the four MOFs were investigated by experimental and molecular simulation strategies, and UiO-66(Zr) was ultimately selected as the sorbent to develop a porous membrane protected micro-solid-phase extraction (μ-SPE) method for simultaneous extraction androgens and progestogens in environmental water samples followed by LC-MS/MS detection. Several variables affecting the extraction efficiency were systematically investigated, including pH, salt concentration, extraction time, kind of desorption solvent, and desorption time. Under the optimized conditions, excellent linearity was obtained in the range of 20.32–2032 ng/L for T, 10.24–1024 ng/L for P, 7.624–762.4 ng/L for TP , and 8.376–837.6 ng/L for MPA . Limits of detection (LODs) and limits of quantification (LOQs) were 10 ng/L and 20 ng/L for T, 4.0 ng/L and 10 ng/L for P, 2.0 ng/L and 7.0 ng/L for TP, and 3.0 ng/L and 8.0 ng/L for MPA, respectively. The recoveries were ranged from 80.5% to 102.4%. Furthermore, the μ-SPE device could be used for at least 10 extractions (RSD < 10.0%). Meanwhile, comparison was made with solid-phase extraction, and the developed method was demonstrated to be a convenient and eco-friendly pretreatment method for water samples.
研究领域:
环境科学
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分析化学
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材料科学
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产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
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IF 3.8
Meiyu Gao,Jiarui Sun,Qinwen Xiao,Yuanyuan Zhai,Yuan Tian,Zunjian Zhang,Fengguo Xu,Pei Zhang
The mevalonate (MVA) pathway plays a crucial role in the occurrence and progression of various diseases, such as osteoporosis, breast cancer, and lung cancer, etc. However, determining all the MVA pathway intermediates is still challenging due to their high polarity, low concentration, chelation effect with metal compartments, and poor mass spectrometric response. In this study, we established a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method coupled with N 2 , N 2 , N 4 , N 4 -tetramethyl-6-(4-(piperazin-1-ylsulfonyl) phenyl)-1,3,5-triazine-2,4-diamine (Tmt-PP) labeling for the simultaneous analysis of all MVA intermediates in biospecimens. Chemical derivatization significantly improved the chromatographic retention, peak shape, and detection sensitivity of the analytes. Moreover, we employed a method named mass spectrum calculation to achieve the absolute quantification of the isomers, i.e., isopentenyl pyrophosphate (IPP) and dimethylallyl pyrophosphate (DMAPP). The established method was fully qualified and applied to explore the difference of these metabolites in cisplatin-resistant non-small cell lung cancer (NSCLC) cells. Additionally, several MVA intermediate analogs, including isopentenyl monophosphate or dimethylallyl monophosphate (IMP/DMAMP), geranyl monophosphate (GMP), 5-triphosphomevalonate (MTP), and isopentenyl triphosphate or dimethylallyl triphosphate (ITP/DMATP), were identified for the first time using a knowledge-driven prediction strategy. We further explored the tissue distribution of these novel metabolites. Overall, this work developed a sensitive quantification method for all MVA intermediates, which will enhance our understanding of the role of this pathway in various health and disease conditions. The novel metabolites we discovered warrant further investigations into their biosynthesis and biological functions.
研究领域:
生物化学
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分析化学
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药理学
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肿瘤学
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代谢组学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
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2023
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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.
研究领域:
食品科学
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农学
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化学
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代谢组学
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茶叶加工
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF ONCOLOGY PHARMACY PRACTICE
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2022
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IF 1.416
Hailong Zhou,Yunyun Li,Fan Xu
PurposeOccupational exposure is a long-standing public health concern, which has drawn more and more attention in recent years to the problem of how to carry out occupational protection effectively. Gloves are regarded as the most critical protective equipment for cytotoxic medications. However, there is still little research conducted on the protective performance of gloves made of different materials and the optimal glove combination for cytotoxic agents.MethodsIn this research, a specific instrument intended for glove permeation experiment was designed, with various methods of liquid chromatography-tandem mass spectrometry (LC-MS/MS) developed and validated. By using the specific instrument and LC-MS/MS methods, a study was conducted on the permeation ability of eight selected cytotoxic drugs (fluorouracil, epirubicin (EPI), docetaxel (DCT), methotrexate (MTX), cyclophosphamide (CTX), etoposide (ETP), vincristine sulfate (VCR), and cisplatin derivatives Pt-(DDTC)3) into five kinds of gloves (rubber (RB), nitrile (NT), chlorinated polyethylene (CPE), low-density polyethylene, and polyvinylchloride (PVC) resin) given different contact times. Then, the experimental data were analyzed through a generalized estimation equation and Pearson correlation analysis.ResultsThe results show that within a short period of time (less than five minutes), ETP, CTX, fluorouracil, DCT, and cisplatin passed through five types of gloves but the level of MTX, VCR, and EPI permeation was minimal, despite the duration of contact between the three drugs and the gloves reaching as long as three hours. Furthermore, the permeation of DCT and ETP was found to be positively correlated with time.ConclusionsChlorinated polyethylene and PVC resin perform well in protecting against most cytotoxic drugs and are recommendable for clinical practice. Due to the poor protective ability, RB gloves are not recommended for this purpose. Based on the performance of various gloves in offering protection, the protection grade of two gloves can be deduced. Chlorinated polyethylene + PVC resin, CPE + NT glove combination shows good protective performance against most target drugs and can be recommended for clinical practice.
研究领域:
药理学
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职业健康
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分析化学
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医学科学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2024
·Vol. 38
·期 6
·e5866
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IF 1.8
Zhijian Zha,Ruihua Wang,Qian Wang,Fahui Chen,Ziyang Ye,Yafeng Li
Immunoglobulin nephropathy (IgAN) stands as the most prevalent primary glomerular nephropathy globally, typically diagnosed through an invasive renal biopsy. Emerging research suggests the significant involvement of chiral amino acids in kidney disease progression. This study introduces a nonderivative LC–tandem mass spectrometry approach, offering efficient separation outcomes within 15 min for identifying chiral amino acids in human urine samples. Subsequently, using this method, the analysis of l - and d -amino acids in the urine of both patients with IgAN and healthy individuals was conducted. Fourteen d -amino acids and 20 l -amino acids were identified in the urine samples obtained from 17 patients with IgAN and 21 healthy individuals. The results indicated notable variances in the concentrations of both l - and d -amino acids between the IgAN and healthy control groups. In contrast to the healthy group, the IgAN group exhibited higher mean urine concentrations of most l -amino acids and lower concentrations of d -amino acids. Furthermore, correlations between amino acids and clinical markers were investigated. These results propose a novel method for monitoring trace amino acids in urine samples and introduce a new concept for potential markers of IgAN.
研究领域:
医学
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分析化学
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肾脏病学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 2
·e6070
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IF 1.7
Li Li,Dan Yu,Wen-Fei Sun,Qi-Zhong Jin,Xing-Jie Chang,Qian Shi
Ginkgolide B (GB) is the main active ginkgolide in Ginkgo biloba leaves extract. Pharmacological study suggested that GB exhibits protective effect on nervous system impaired and can be used in the treatment of dementia, cerebral insufficiency or related cognitive decline. However, the information on pharmacokinetics of GB in vivo was limited. In this study, a sensitive LC–MS/MS analytical method was developed to accurately determinate the concentration of GB in dog plasma and applied to the pharmacokinetic study of GB in dogs after bolus injection of GB. A portion of 100 μL dog plasma was pretreated by liquid–liquid extraction using 1 mL of ethyl acetate. The GB and IS were separated on a Waters ACQUITY HSS T3 column using acetonitrile and water containing 0.1% formic acid as mobile phase, at a flow rate of 0.4 mL/min. Multiple-reaction monitoring (MRM) mode was used for quantitative analysis of GB and tolbutamide (internal standard) in negative electrospray ionization. GB showed excellent linearity with correlation coefficient > 0.99 over the concentration range of 1–5000 ng/mL. The intra and interday RSD% were less than 7.4%, while the RE% ranged from −6.1% to 9.6%. The mean extraction recovery was > 83.1%. The validated method was further successfully applied to pharmacokinetic study of GB in dog plasma. Dose-proportional pharmacokinetics of GB were observed after bolus injection administration in dogs. This comprehensive study of the pharmacokinetics of GB in dogs will provide useful information for its further development in clinic.
研究领域:
药理学
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分析化学
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产品关联
DOI
PubMed
高影响因子
Pharmacology Research & Perspectives
·
2025
·Vol. 13
·期 3
·e70126
·
IF 2.3
Yuanxia Yang,Yue Zhang,Yingdong Qu,Liwan Cui
Sirolimus is a third-generation immunosuppressant with multiple efficacies, including antifungal, antitumor, and immunosuppressive properties. We conducted a pharmacokinetic study to determine the effect of berberine hydrochloride (BBR) on the pharmacokinetics of sirolimus in rats. Thirty-six rats were randomly divided into six groups, and blood samples were collected from the posterior orbital venous plexus at different time points after the last administration to determine the plasma concentration of sirolimus. Liquid chromatography tandem mass spectrometry (LC–MS/MS) was used for detection, and DAS 2.0 software was employed for pharmacokinetic analysis. A single administration of BBR significantly reduced the pharmacokinetic parameter AUC 0-12h of sirolimus. Repeated administration of BBR resulted in an upward trend in C max AUC 0-12h , AUC 0-∞ , and CLz all show an upward trend. This study indicates that BBR has a certain impact on the pharmacokinetics of sirolimus in rats. However, further validation of the role of gene polymorphism in pharmacokinetics and clinical efficacy is needed for further research in a wider population.
研究领域:
药理学
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免疫学
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产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2014
·Vol. 6
·期 21
·8713-8721
·
IF 1.938
Feng Chen,Hai-Long Li,Yin-Feng Tan,Wei-Yong Lai,Zhen-Miao Qin,Hong-Die Cai,Yong-Hui Li,Jun-Qing Zhang,Xiao-Po Zhang
Euscaphic acid, a triterpene acid, exists ubiquitously in medicinal plants and demonstrates various pharmacological activities. This active compound is often used as a marker compound for quality control. Hitherto, the pharmacokinetic (PK) information is relatively scarce; therefore, it remains open to question whether the euscaphic acid reaches the target sites in the body at concentrations high enough for the claimed biological effects. A robust analytical method is prerequisite for obtaining enough PK information of euscaphic acid, which is useful for interpreting its pharmacological effects. In this study, we developed and validated a rapid liquid chromatographic tandem mass spectrometric (LC-MS/MS) method for the measurement of euscaphic acid in rat plasma. The rat plasma samples were precipitated with acetonitrile and the resulting supernatants were separated by a 4 min pulse gradient method on a Synergi Fusion-RP C18 column (4 μm, 2.0 mm i.d. × 50 mm). Ursolic acid was used as an internal standard for quantification of euscaphic acid. Deprotonated euscaphic acid and its internal standard were generated in negative electrospray ionization (ESI) mode and their precursor-to-product ion pairs (m/z 487.4→469.3 and 455.5→455.4, respectively) were used for measurement. Notably, the commonly used concentration of formic acid (HCOOH; 1‰ and 5‰, v/v) in the mobile phase seriously suppressed the signal intensity, but this mobile phase additive at a much lower concentration level (0.1‰ and 0.2‰) could overcome the matrix effects and therefore increase the sensitivity of MS detection of euscaphic acid. The newly developed bioanalytical assay possessed favorable accuracy and precision with a lower limit of quantification of 2.0 ng mL−1 and was successfully applied to PK studies in rats. The experimental strategies presented herein may be helpful for measurement of other triterpene acids in biological matrices.
研究领域:
分析化学
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药理学
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生物医学
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产品关联
DOI
高影响因子
ANALYTICA CHIMICA ACTA
·
2021
·
IF 6.558
Ruiqin Zhu,Hang Mei,Huajing Liu,Changbao Hong,Xiantao Shen,Chuixiu Huang
Practical biological and environmental samples always contain both acidic and basic substances, and the samples are always precious. Thus, separation of analytes with different nature from the same sample was of great significance. Successive liquid phase microextraction (sLPME) of acidic and basic analytes under optimal extraction conditions was therefore proposed for the first time. The concept of sLPME was proved by using three acidic analytes (naproxen, flurbiprofen and diclofenac) and three basic analytes (haloperidol, fluoxetine and sertraline) as model analytes, and using polypropylene glycol with an average molecular weight of 4000 (PPG4000) as SLM . The recoveries of all target analytes by sLPME were similar to that by individual LPME due to good affinity of PPG4000 to both acidic and basic analytes. Under optimal extraction conditions, the recoveries for all analytes by sLPME from urine samples were in the range of 62%–95%. Moreover, combined with LC-MS/MS, such sLPME approach was also evaluated with urine samples. The matrix effect of sLPME-LC-MS/MS at different levels for all analytes ranged from −14.1%–13.2%. The linear ranges with R 2 > 0.996 were 5–1000 ng mL −1 for basic analytes, and 20–1000 ng mL −1 for acidic analytes except diclofenac (1–1000 ng mL −1 ). The repeatability and accuracy at four levels were in the range of 3%–10% and 86%–120%, respectively. The limit of detection (LOD, S/N = 3) and limit of quantification (LOQ, S/N = 10) were found to be 0.07–0.49 ng mL −1 and 0.25–1.63 ng mL −1 , respectively. Finally, the strategy for constructing a sLPME system was further confirmed with urine, plasma and saliva using another two versatile SLM solvents possessing high affinity to both acidic and basic analytes. Successive LPME enabled separation of acidic and basic analytes from the same sample under optimum extraction conditions for all target analytes. Thus, we believe that the sLPME system will become a potent platform for forensic toxicology analysis, food science, environmental analysis and epidemiology study.
研究领域:
分析化学
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环境科学
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法医学毒理学
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产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2021
·Vol. 13
·期 38
·4515-4527
·
IF 2.896
Zheng Gao,Ruizhi Tang,Shujuan Ma,Shicong Jia,Shuai Zhang,Bolin Gong,Junjie Ou
Although macroporous adsorbent resins (MARs) have been commercialized and widely applied in industrial and life fields, it is still of necessity to develop simple approaches to functionalize MARs. One of the most widely used methods to realize excellent fouling resistance performance is surface modification of hydrophilic polymers on substrates to fabricate an anti-biofouling coating. Herein, three kinds of hydrophilic poly(glycidyl methacrylate-co-ethylene glycol dimethacrylate) MAR were designed and facilely prepared by coating a layer of porous organic polymers (POPs) via either an epoxy–amine ring-opening polymerization or amine–aldehyde condensation reaction using isophthalaldehyde (IPA), 1,4,7,10-tetraazacyclododecane (cyclen), melamine and 1,3,5-triglycidyl isocyanurate (TGIC) as precursors. By taking advantage of their merits, such as large surface area, excellent hydrophilicity and unbiased affinity toward all types of glycopeptide, three functionalized hydrophilic MARs were successfully applied to capture glycopeptides from complex samples as hydrophilic interaction liquid chromatography (HILIC) sorbents. A total of 694 N-glycopeptides and 372 N-glycosylation sites were identified from 2 μL of human serum digest with poly(TC)@MAR, which were not only more than those of poly(MT)@MAR (286 N-glycosylation sites and 547 N-glycopeptides) and poly(IM)@MAR (669 N-glycopeptides and 355 N-glycosylation sites), but also more than those of other reported HILIC materials. This work provided a new and simple way to synthesize enrichment materials for liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) analysis of glycoproteomes.
研究领域:
生物化学
·
分析化学
·
蛋白质组学
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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）