BIOMEDICAL CHROMATOGRAPHY
·
2024
·Vol. 38
·期 6
·e5866
·
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
·
分析化学
·
肾脏病学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 2
·e6070
·
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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DOI
PubMed
高影响因子
JOURNAL OF FOOD BIOCHEMISTRY
·
2022
·Vol. 46
·期 8
·e14204
·
IF 3.654
Tao Liu,Xingze Cao,Dongmin Cao
Osteoarthritis (OA) is a disabling disease and seriously affects the quality of life of patients. is A potential medicine for the treatment of OA is Eucommia ulmoides leaves (EULs). However, its active compounds and therapeutic mechanisms are unclear. Therefore, it is necessary to develop a method using LC–MS and network pharmacology for the detection and identification of compounds and the mechanisms of action of EULs. The compounds were detected and identified based on ultra-high-performance liquid chromatography coupled with Quadrupole Exactive-Orbitrap MS (UHPLC-Q Exactive-Orbitrap MS) and followed by the network pharmacology analysis. Seventy-three compounds, including 15 flavonoids, 8 iridoids, 10 lignans, 24 phenolic acids, and 16 additional compounds, were identified by UHPLC-Q Exactive-Orbitrap MS. The network of the pharmacological analysis revealed that 29 active compounds regulated 17 main pathways through 38 target genes, including NF-kappa B signaling pathway, PI3K-Akt signaling pathway, AMPK signaling pathway, etc. In conclusion, EULs were effective in the treatment of OA by regulating the abovementioned key pathways. This study showed that LC–MS/MS followed by network pharmacology analysis is useful to elucidate the complex mechanisms of action of Chinese herb. Practical applications This study describes a rapid method of detecting and identifying the constituents and systematic mechanism of Eucommia ulmoides based on LC–MS and network pharmacology. Our results show that 73 compounds of E. ulmoides leaves were identified and predicted that E. ulmoides leaves were effective in the treatment of OA by regulating key pathways, including NF-kappa B signaling pathway, PI3K-Akt signaling pathway, and AMPK signaling pathway by network pharmacology, which lays the foundation for subsequent research.
研究领域:
中药学
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分析化学
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分子生物学
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2017
·
IF 2.603
Wenhua Li,Bin Yang,Dongmei Zhou,Jun Xu,Wenjia Li,Wen-Chen Suen
Sodium dodecyl sulfate capillary electrophoresis (CE-SDS) has been widely used to separate and quantify monoclonal antibody (mAb) fragments and impurities. Two fragments with different masses smaller than monomer were observed in the CE-SDS analysis of a recombinant IgG1 mAb treated at 40 °C for 28 days. Reversed phase liquid chromatography mass spectrometry (RP–LC–MS) and trypsin digestion peptide mapping followed by LC–MS/MS analysis were employed to conclusively demonstrate that these antibody fragments were the degradation products derived from a Ser–Ser peptide bond cleavage at the heavy chain complementarity determining region (CDR). The total percentage of the cleaved antibody heavy chain was increased from 1.1% in the control sample to 4.6% in the forced degradation sample stored at 40 °C for 28 days by using CE-SDS analysis. Native size exclusion liquid chromatography (SEC-HPLC) was used to analyze the fragment profile of this treated mAb but did not reveal fragments smaller than the monomer. However, a small fragment was detected using denaturing size exclusion liquid chromatography (dSEC-HPLC) and was confirmed to be the N-terminal fragment of the heavy chain cleaved at the CDR region using RP–LC–MS analysis. These results suggested that this N-terminal fragment may be closely associated with the rest of the cleaved antibody molecule through non-covalent bond interactions. Moreover, when dSEC-HPLC and RP–LC–MS were used to analyze the aggregate and monomer samples individually collected from SEC-HPLC, both samples contained the same amount of the cleaved N-terminal fragment. These results suggested that the CDR region cleaved fragments likely not be involved in aggregates formation of this antibody. This case study reiterated that a combination of orthogonal analytical methods plays a crucial role in comprehensively analyzing and characterizing antibody fragmentation.
研究领域:
生物化学
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分析化学
·
蛋白质组学
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DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Juan Liu,BiYa Gong,Ping Zhang,JuanJuan Wu,Chun Yi,ChunMei Wang,YouHan Kong
Chinese bayberry ( Morella rubra Lour ) is a fruit from the Myricaceae family, rich in various dietary nutrients, and has a long history of cultivation and use in both food and medicine. The diversity of Chinese bayberry resources and its perishable nature limit its reprocessing and long-distance sales, posing challenges for the industry. This study compared the decay resistance characteristics, soluble solids, organic acids, and apparent traits of six different Chinese bayberry resources in Hunan Province, evaluating their edibility and processing characteristics. Using LC-MS and GC–MS, the non-volatile and volatile components of the six types of Chinese bayberry were extensively identified. The results showed that different types of Chinese bayberry contain distinct metabolites, which are significantly correlated with their decay resistance and apparent traits. Compounds such as Mesuagin, Arctigenin, and Eugenin were directly related to the decay area ratio and fruit weight. Licoricidin and Naringenin may have potential relationships with decay resistance. In this study, we took bayberry from six different resources as an example and preliminarily demonstrated that there were significant differences in the decay resistance and apparent traits of different bayberry varieties, which were related to their internal metabolites. Several specific substances in bayberry that are directly related to the preservation and reprocessing characteristics of bayberry were identified. These substances may have the potential to become key potential markers for evaluating the processing and storage characteristics of bayberry.
研究领域:
食品科学
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植物化学
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代谢组学
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DOI
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
·
免疫学
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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
·
药理学
·
生物医学
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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
·
环境科学
·
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
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分析化学
·
蛋白质组学
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产品关联
DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2021
·
IF 6.558
Qianqian Shang,Hang Mei,Xinrui Feng,Chuixiu Huang,Stig Pedersen-Bjergaard,Xiantao Shen
Electromembrane extraction (EME), involving the migration of charged analytes across a supported liquid membrane (SLM) with an external power supply, is a promising sample preparation method in analytical chemistry . However, the presence of boundary double layers at the SLM/solution interfaces often restricts extraction efficiency. To avoid this, the current work proposed an ultrasound-assisted EME (UA-EME) method based on a novel type of supported semi-liquid membrane (SsLM). The characterizations showed that the SsLM was stable under ultrasound conditions. Ultrasound was found to reduce the boundary double layers and thus increase the mass transfer. Major operational parameters in UA-EME including ultrasound power density, temperature, applied voltage and extraction time were optimized with haloperidol , fluoxetine , and sertraline as model analytes. Under the optimal conditions, extraction recoveries of model analytes in water samples were in the range of 66.8%–91.6%. When this UA-EME method was coupled with LC-MS/MS for detection of the target analytes in human urine samples, the linear range of the analytical method was 10–1000 ng mL −1 , with R 2 > 0.997 for all analytes. The limits of detection (LOD) and limits of quantification (LOQ) were in the range of 1.7–2.1 ng mL −1 and 5.7–6.7 ng mL −1 , respectively. The UA-EME expands the application field of ultrasound chemistry and will be very important in development of stable and fast sample preparation systems in the future.
研究领域:
分析化学
·
超声化学
·
药物分析
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2022
·Vol. 61
·期 2
·130-139
·
IF 1.555
Sun Lu-Ning,Shen Ye,Yang Yu-Qing,Chen Xiang-Long,Huang Feng-Ru,Wang Dun-Jian,Zhang Ye,Wang Da-Wei,Wang Yong-Qing
The feasibility of taking the ratio of 6β-hydroxycortisol (6β-OHCOR) to cortisol (COR) in plasma as a biomarker to reflect CYP3A4 activity needs to be verified, but the low concentration of 6β-OHCOR which is an endogenous substance in plasma presents a challenge for determination. In this study, a Liquid chromatography with tandem mass spectrometry (LC–MS/MS) method was established to simultaneously quantify the COR and 6β-OHCOR in plasma with COR-d4 and 6β-OHCOR-d4 as internal standards (ISs). Plasma samples were treated by protein precipitation using acetonitrile. Separation with a gradient elution within 5 min was achieved on C18+ column utilizing 5 mM ammonium formate and methanol. An API 4,000 MS in multiple reaction monitoring mode with transitions of 407.1 → 361.1 and 423.1 → 347.1 was utilized. Albumin solution was used as a surrogate matrix, with good linearities over the concentration of 1.20–300 ng/mL for COR and 0.0400–10.0 ng/mL for 6β-OHCOR. The precisions for intrarun and interrun were < 6.8%, and the accuracy was fell in the interval of −5.2 to 3.5%. Matrix effect was not found. Recovery was close to 100.0%. Stability was confirmed under the storage and processing conditions. The validated method was applied to evaluate the inhibitory effect of voriconazole to CYP3A by the ratio of 6β-OHCOR to COR.
研究领域:
分析化学
·
药理学
·
临床医学
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产品关联
DOI
PubMed
高影响因子
BIOCHIMICA ET BIOPHYSICA ACTA-GENERAL SUBJECTS
·
2022
·
IF 4.117
Tan Qin,Yu Wang,Jing Nie,Lushan Yu,Su Zeng
Background Sodium taurocholate co -transportering polypeptide (NTCP, SLC10A1 ) is a vital bile acid transporter and the functional receptor of hepatitis B and D virus. The oligomerization of NTCP is important for the structural study of its interaction with HBV preS1 peptide. Methods Recombinant NTCPs were expressed in Sf9 host cell using baculoviruses. Function of recombinant NTCP was verified by liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) method. A quantitative fluorescence resonance energy transfer (FRET) method was established to analyze the interaction between NTCP wild type (WT) and mutants. Co-immunoprecipitation (Co-IP) was used to test the interaction between NTCP variants. Results Sub-cellular location of recombinant NTCPs varies with the modification of NTCP. Bands of monomer, dimer and oligomers were shown in gel analysis of NTCP. Significant FRET was observed between cyan florescence protein (CFP) tagged NTCP and yellow florescence protein (YFP) tagged NTCP. FRET efficiency between CFP- and YFP-NTCP S267F mutants was lower than WT. Co-IP results showed that S267F interacts with WT NTCP when co-expressed in cell. Conclusion Dimer is the predominant form of NTCP expressed in Sf9 when solubilized with detergent. FRET and Co-IP analysis support that NTCP forms oligomers in Sf9 cell. General significance Our results showed that NTCP formed oligomers in Sf9 cell. Meanwhile the FRET analysis of NTCP variants further elucidated the molecular mechanism of NTCP oligomerization.
研究领域:
病毒学
·
分子生物学
·
细胞生物学
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DOI
PubMed
高影响因子
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