JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Yu Zhonghao,Yuan Yuhao,Zhang Jiaxin,Tao Jing,Gao Hang,Gao Xiangting,Zhou Yiwu
Insulin, a peptide hormone essential for blood glucose regulation, is typically quantified in clinical practice using immunoassays. While sensitive, these assays lack specificity and are often inadequate for the precise qualification and quantification in forensic practices. To address this limitation, we developed and validated an LC-Orbitrap-HRMS method for the quantification of intact insulin and its analogues in four postmortem matrices: plasma, liver, kidney, and adipose tissue. Method validation demonstrated linearity for human insulin in plasma from 0.1 to 100 ng/mL, with accuracy between 90.1 % and 106.9 %. Notably, in challenging matrices such as adipose tissue, the LLOQ was 1 ng/mL, with accuracy range from 94.1 % to 100.2 %, confirming robust analytical performance. The validated method was applied on two forensic cases involving suspected insulin overdose. Insulin concentrations in subcutaneous adipose tissue from the injection sites were significantly elevated, measuring 743.1 ng/mL and 53.2 ng/mL, respectively. These results demonstrate the utility of the method in providing reliable evidence for the investigation of suspected fatal insulin intoxication.
研究领域:
分析化学
·
法医学
·
毒理学
·
药物分析
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内分泌学
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PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2026
·Vol. 49
·期 2
·e70366
·
IF 3.6
Hangming Li,Tianqi Ma,Guoqing Jin,Shenghong Guan,Jiaye Li,Ping Huang,Xueli Hu,Shuxin Chen,Zhao Wang,Jingkui Tian,Shouxin Li,Xiaoyong Zhang
Shaoyao Ruangan Decoction (SYRGD), a classic traditional Chinese medicine (TCM) preparation composed of over a dozen herbs, is widely used in the clinical treatment of liver cancer, hepatitis, and liver cirrhosis. In this study, we elucidated the chemical basis of SYRGD and, for the first time, its in vivo metabolic pathways and dynamic gastrointestinal changes by combining ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-Q-Orbitrap-MS/MS) with the Simulator of the Human Intestinal Microbial Ecosystem (SHIME) model. Results revealed the identification of 101 constituents in SYRGD, primarily including flavonoids, terpenoids, organic acids, and alkaloids. Within the SHIME digestive fluids, 69 prototype components and 67 metabolites were identified, with the metabolic pathways primarily involving hydroxylation, oxidation, sulfation, and glucuronidation. Dynamic analysis showed that most prototype components were gradually absorbed or transformed, exhibiting a decreasing concentration gradient from the stomach to the colon. In contrast, many metabolites showed significant enrichment in the stomach and small intestine prior to their absorption or further transformation, indicating that metabolic reactions occurred throughout the entire digestive process. This study provides a comprehensive reference for the clinical application and further development of SYRGD. The systematic methodology is rapid, reproducible, overcomes the limitations of conventional animal or clinical trials, and establishes a precise research strategy for investigating the metabolism of other complex herbal medicines.
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高影响因子
Analytical Methods
·
2022
·Vol. 14
·期 47
·4990-5000
·
IF 3.532
Xiangyu Zhang,Yaojuan Chu,Mengli Wang,Yingying Shi,Lihua Zuo,Zhuolun Li,Jiyun Liu,Jian Kang,Shuzhang Du,Bing Li,Zhi Sun,Xiaojian Zhang
Mai-Luo-Shu-Tong pill is an effective traditional Chinese medicine formula for the treatment of superficial thrombophlebitis, but it was insufficiently chemically scrutinized. In this study, the mass spectral data of Mai-Luo-Shu-Tong pill were acquired by ultra-high performance liquid chromatography coupled with Q Exactive hybrid Quadrupole-Orbitrap high resolution mass spectrometry. Then, a data mining strategy combining multiple data processing methods was used to identify chemical constituents in Mai-Luo-Shu-Tong pill by constructing a database of precursor ions and summarizing the mass spectral fragmentation behaviors. As a result, a total of 211 compounds including 70 flavonoids, 56 terpenoids, 37 phenolic acids and 48 others were identified in positive and negative ion modes. Among them, 66 compounds have passed comparison verification with reference standards, 145 compounds were identified based on the data mining strategy combining the characteristic cleavage behaviour of homologous compounds and fragment ions and 4 compounds were potentially new compounds. This study provides a database for quality evaluation and further study of Mai-Luo-Shu-Tong pill in vivo. Moreover, it provides a reference for the characterization of the chemical constituents of other traditional Chinese medicine formulae.
研究领域:
中药化学
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分析化学
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药学
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DOI
高影响因子
CURRENT DRUG METABOLISM
·
2021
·Vol. 22
·期 1
·70-82
·
IF 3.731
Zuo Lihua,Li Jia,Xue Lianping,Jia Qingquan,Li Zhuolun,Zhang Mengya,Zhao Mengfan,Wang Mengli,Kang Jian,Du Shuzhang,Sun Zhi
Background: Alpiniae oxyphyllae Fructus (AOF), a traditional Chinese medicine (TCM), is widely used in the treatment of urinary, gastrointestinal and neurologic diseases in China. Although terpenoids are the main active ingredients of AOF, there are few researches on their pharmacokinetics
and metabolism. Methods: In this study, a sensitive, rapid, accurate and novel ultra high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was established to evaluate the pharmacokinetic behavior of five terpenoids (oxyphyllenodiol B, (4S* ,5E,10R*)-7-oxo-tri-nor-eudesm-5-en-4β-ol,
7-epi-teucrenone, (+)- (4R,5S,7R)-13-hydroxynootkatone, (E)-labda-12,14-dien-15(16)-olide-17-oic acid) in rats after oral administration of AOF extracts. 27 metabolic metabolites of the five terpenoids were identified by ultra high performance liquid chromatography -Q Exactive hybrid quadrupole-orbitrap
high-resolution accurate mass spectrometry (UHPLC-Q-Orbitrap HRMS) based on precise mass and fragment ions. Results: The established pharmacokinetic analysis method showed good linearity over a wide concentration range, and the lower quantitative limit (LLOQ) ranged from 0.97 to 4.25
ng/mL. Other validation parameters were within the acceptable range. In addition, 27 metabolites were identified in plasma, urine and feces samples, and the metabolic pathways of five terpenoids were mainly focused on glucoside conjugation, dehydration, desaturation and glycine conjugation.
Conclusion: This is the first study on the pharmacokinetics and metabolism of five terpenoids in AOF, illuminating the disposal process of terpenoids in vivo. It was expected that the results of this study would provide some references for the apprehension of the action mechanism and
the further pharmacological study of five terpenoids in AOF.
研究领域:
中药学
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分析化学
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药理学
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DOI
高影响因子
JOURNAL OF MASS SPECTROMETRY
·
2026
·Vol. 61
·期 8
·e70087
·
IF 2.1
Hanting Li,Liangyin Shu,Suyu Yang,Qing Li,Huanting Li,Wei Cai,Shunli Xiao
Solanum virginianum L., a traditional Solanaceae medicinal plant, is clinically valued for dispelling wind-dampness and relieving pain. Previous phytochemical investigations have predominantly focused on the fruits, identifying alkaloids and steroids with notable anti-inflammatory and antipsoriasis activities. However, systematic research regarding the chemical constituents of other medicinal parts, such as roots and stems, remains scarce, hindering a comprehensive understanding of the plant's material basis. To address this gap, this study systematically characterizes the chemical components of different parts leaves-stems, roots, and fruits-providing essential data for the holistic utilization and quality control of S. virginianum . The chemical constituents of S. virginianum . were fully investigated using Ultra-High Performance Liquid Chromatography-Quadrupole-Exactive Orbitrap Mass Spectrometry (UHPLC-Q-Exactive Orbitrap MS) combined with the Feature-based molecular networking (FBMN). A total of 110 chemical components were identified by comparison with reference standards, databases, and literature. Among them, 89 compounds were reported for the first time in this species, 18 compounds were accurately confirmed, and 51 compounds were simultaneously identified in all three parts, leaves-stems (L), roots (R), and fruits (F). The established method enables rapid and effective identification of the main chemical constituents in S. virginianum , providing a reference for its quality control, studies on active components, and mechanism of action exploration.
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高影响因子
FOOD RESEARCH INTERNATIONAL
·
2025
·
IF 8
Huan-ya Yang,Lin Yang,Yu-lu Wang,Yun-shu Hu,Yun Li,Hua Qu,Wen-long Wei,Hui-yan Yang,Qi-rui Bi,Jian-qing Zhang,De-an Guo
Ginger is extensively utilized in culinary and traditional medicine worldwide. This study presents a comparative analysis on ginger-related varieties from different species, growth stages, processing methods and geographical origins using headspace solid-phase microextraction gas chromatography quadrupole time-of-flight mass spectrometry (HS-SPME-GC-Q-TOF MS) and ultra-high performance liquid chromatography linear-ion-trap-quadrupole orbitrap MS (UHPLC-LTQ-Orbitrap MS). A total of 120 volatiles and 377 non-volatiles were annotated. Metabolomics revealed 44 differential components to discriminate six Zingiberaceae species. Among them, ginger contained the highest levels of chemical components. Additionally, 44 components were found to completely distinguish two growth stages and four processing forms of ginger. As ginger matures, changes in volatiles become more pronounced, while significant differences in non-volatiles were observed across processing stages. Moreover, ginger from three regions was compared, and ginger from Western was found to have more abundant non-volatiles and a higher qualification rate (Yunnan 100 % vs. Fujian 33 %, Henan 15 %). This study maps the chemical profile of ginger and related varieties, providing insights for development of novel products and informing decisions in cultivation, production, and purchasing.
研究领域:
植物化学
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食品科学
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药用植物学
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PubMed
高影响因子
MOLECULES
·
2024
·Vol. 29
·期 18
·4349
·
IF 4.2
Yanghui Huo,Kailin Li,Suyu Yang,Bo Yi,Zhihua Chai,Lingxuan Fan,Liangyin Shu,Bowen Gao,Huanting Li,Wei Cai
The traditional Mongolian medicine Erdun-Uril is a conventional combination of 29 herbs commonly used for the treatment of cerebrovascular ailments. It has the effects of reducing inflammation, counteracting oxidative stress, and averting strokes caused by persistent cerebral hypoperfusion. Prior research on Erdun-Uril has predominantly concentrated on its pharmacodynamics and mechanism of action; however, there has been a lack of systematic and comprehensive investigation into its chemical constituents. Therefore, it is crucial to establish an efficient and rapid method for evaluating the chemical constituents of Erdun-Uril. In this study, Erdun-Uril was investigated using UHPLC-Q-Exactive Orbitrap MS combined with parallel reaction monitoring for the first time. Eventually, a total of 237 compounds, including 76 flavonoids, 68 phenolic compounds, 19 alkaloids, 7 amino acids, etc., were identified based on the chromatographic retention time, bibliography data, MS/MS2information, neutral loss fragments (NLFs), and diagnostic fragment ions (DFIs). And of these, 225 were reported for the first time in this study. This new discovery of these complex components would provide a reliable theoretical basis for the development of pharmacodynamics and quality standards of the Mongolian medicine Erdun-Uril.
研究领域:
药理学
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分析化学
·
传统医学
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DOI
PubMed
高影响因子
Heliyon
·
2024
·
IF 3.4
Ruijie Li,Haoliang Ke,Pan Liu,Qian Yang,Yuxin Li,Longzhu Ke,Xiuping Wang,Chaoyan Wu,Yingwen Zhang
Ethnopharmacological relevance Yiai Fuzheng formula (YAFZF), as a Traditional Chinese Medicine (TCM) prescription, has been used widely at Zhongnan Hospital of Wuhan University for its therapeutic effects and high safety on triple-negative breast cancer (TNBC). Objective In this study, we employed ultra-high-performance liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometry (UPLC-Q-Orbitrap-HRMS), network pharmacology, and experimental validation to elucidate the underlying action mechanism of YAFZF in the treatment of TNBC. Methods The key active ingredients in YAFZF were analyzed using UPLC-Q-Orbitrap-HRMS, and then the potential components, target genes and signalling pathways of YAFZF were predicted using the network pharmacological method. We then used molecular docking to visualize the combination characteristics between major active components and macromolecules in the crucial pathway. In vitro experiments were conducted to investigate the inhibitory effects of YAFZF treatment on the cell viability, invasion, and migration of 4T1 and MDA-MB-231 cells. The xenograft TNBC models were constructed using female Balb/c mice, and their body weights, tumour volumes, and weights were monitored during YAFZF treatment. Quantitative real-time PCR (qRT-PCR), Hematoxylin-eosin (HE), immunohistochemistry (IHC) staining, Western blot (WB), and terminal deoxynucleotidyl transferase (TdT)-dUTP nick-end labeling (TUNEL) staining were used for further experimental validation. Results Based on UPLC-Q-Orbitrap-HRMS and network pharmacology analysis, 6 major bioactive components and 153 intersecting genes were obtained for YAFZF against TNBC. Functional enrichment analysis identified that the phosphatidylinositol 3-kinase (PI3K)-protein kinase B (Akt) signalling pathway might be the mechanism of action of YAFZF in the treatment of TNBC. Molecular docking results suggested that the main active compounds in YAFZF had strong binding energies with the proteins in the PI3K/Akt pathway. In vitro experiments showed that YAFZF inhibited the cell viability, invasion, and migration abilities of TNBC cells. Animal experiments confirmed that YAFZF treatment suppressed tumour cell proliferation and increased apoptotic cells. PCR, HE, WB, and IHC results indicated that YAFZF could suppress xenograft tumour metastases by inhibiting the PI3K/AKT/mTOR pathway regulating the epithelial-mesenchymal transition (EMT) process. Conclusion YAFZF therapy showed its potential for reducing proliferation, invasion, and migration abilities, increasing apoptosis of TNBC cells. Furthermore, YAFZF treated TNBC by inhibiting xenograft tumour distant metastases via the regulation of EMT by the PI3K/Akt/mTOR pathway, suggesting that it may be useful as an adjuvant treatment.
研究领域:
药理学
·
肿瘤学
·
中医药
·
分子生物学
·
癌症研究
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PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2021
·
IF 3.935
Qingkun Ma,Chao Qi,Xi-Ling Li,Qing Shi,Chun-Yan Xu,Toufeng Jin,Jun Zhe Min
A high-sensitivity and -selectivity mass spectrometry derivatization reagent, ( R )-(5-(3-isothiocyanatopyrrolidin-1-yl)-5-oxopentyl) triphenylphosphonium (NCS-OTPP), was developed for the enantiomeric separation of chiral thiol compounds as prospectively important diagnostic markers for oxidative stress-related diseases. Complete separation of GSH, DL-Cys, and DL-Hcy was achieved. The parent ions of all derivatives had a fragment of m/z 473.18 and a structure of m/z 75.95 (R-S = C-S-R’), conducive to qualitative and quantitative analysis. Good linear relationships were obtained for all analytes ( R 2 ≥ 0.9995). The intra-day and inter-day precision were 0.82–5.16 % and 1.02–4.18 % in saliva, and 0.81–3.45 % and 0.99–6.47 % in urine, with mean recoveries of 83.31–105.66 % and 84.09–101.11 %, respectively. The limit of detection ( S/N = 3) was 19.20–57.60 nM. Free and total GSH, DL-Cys, and DL-Hcy were detected simultaneously in saliva and urine from 10 volunteers in the normal, stressed, and stable states by UHPLC-Q-Orbitrap HRMS . The thiol compounds were quantitatively related to oxidative stress state changes.
研究领域:
分析化学
·
医学
·
生物化学
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产品关联
DOI
PubMed
高影响因子
Frontiers in Pharmacology
·
2019
·
IF 3.845
Sun Zhi,Yang Jie,Liu Liwei,Xu Yanyan,Zhou Lin,Jia Qingquan,Shi Yingying,Du Xiangyu,Kang Jian,Zuo Lihua
Trepibutone was widely used for cholelithiasis, cholecystitis, biliary tract dyskinesia, cholecystectomy syndrome, and chronic pancreatitis in clinic. However, few investigations on trepibutone have been conducted. In this study, an accurate, sensitive, and selective analytical method was developed and successfully applied to assess the pharmacokinetic behavior of trepibutone in rats. Trepibutone and carbamazepine (internal standard, IS) were quantified using multiple reaction monitoring (MRM) mode with the transitions of m/z 311.09→265.08 and m/z 237.06→194.08, respectively. The linearity, precision, accuracy, extraction recovery, matrix effect, and stability of the established method were all excellent within acceptable range. A total of 30 metabolites were identified in plasma and urine by Q-Exactive high resolution mass spectrometry, and several common metabolic pathways were observed such as dealkylation, oxidation, reduction, glucuronidation, and so on. This research provides more information on trepibutone in pharmacodynamics and toxicology and will assist the usage of trepibutone in clinical.
研究领域:
药物代谢
·
临床药理学
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分析化学
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DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2017
·Vol. 40
·期 22
·4453-4466
·
IF 2.557
Zhi Sun,Zhuolun Li,Lihua Zuo,Zhenhui Wang,Lin Zhou,Yingying Shi,Jian Kang,Zhenfeng Zhu,Xiaojian Zhang
To clarify and quantify the chemical profile of YiXinShu Tablet rapidly, a feasible and accurate strategy was developed by applying ultra high performance liquid chromatography with Q Exactive hybrid quadrupole orbitrap high-resolution accurate mass spectrometry. A total of 105 components were identified, including 25 phenanthraquinones, 11 lactones, 19 lignans, 24 acids, and 26 other compounds. Among them, 26 major compounds were unambiguously detected by comparing with reference standards. And 19 of these compounds in three batches of YiXinShu Tablet were selected for quantitative determination. ( Z )-Ligustilide, salvianic acid A, salvianolic acid A, salvianolic acid B, and rosmarinic acid were abundant in these three batches with contents over 1 mg/g. The established analysis methods were examined to be accurate and feasible. The results show that the ultra high performance liquid chromatography with Q Exactive hybrid quadrupole orbitrap high-resolution accurate mass spectrometry method has a powerful qualitative ability and promising quantitative application.
研究领域:
分析化学
·
药学
·
质谱分析
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PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2023
·
IF 6.2
Xi-Ling Li,Yuxuan Li,Shuyun Xiao,Qingsong Li,Chengqiang Han,Danyang Liu,Tengfei Cui,Xiyang Rao,Kenichiro Todoroki,Guang Yang,Jun Zhe Min
Acute myocardial infarction (AMI) poses a grave threat to human life. However, most clinical biomarkers have limitations of low sensitivity and specificity. Therefore, screening novel glycan biomarkers with high sensitivity and specificity is crucial for the prevention and treatment of AMI. The novel method of ultrahigh-performance liquid chromatography coupled to quadrupole-Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) with d0/d5-BOTC probe labeling for relative quantification of glycans based on Pronase E digestion was established to screen novel glycan biomarkers in the serum of 34 AMI patients relative to healthy volunteers. The monosaccharide model D-glucosamine was used to investigate the effectiveness of the derivatization ; the limit of detection (S/N = 3) was 10 amol. The accuracy was verified based on the consistency of different theoretical molar ratios (d0/d5 = 1:2, 2:1) and intensity ratios following digestion of glycoprotein ribonuclease B. Expressions of H4N4F3SA, H4N6F2, H4N6SA, H4N6F3 and H5N4FSA in the serum were significantly different ( p < 0.0005) between AMI patients and healthy volunteers. The area under the receiver operating characteristic curve (AUC) for H4N6SA, H5N4FSA, and H4N6F2 was greater than 0.9039. Based on the proposed method, H4N6SA, H5N4FSA, and H4N6F2 in human serum showed high accuracy and specificity and may serve as potential glycan biomarkers, crucial for the diagnosis and treatment monitoring of AMI.
研究领域:
医学
·
分析化学
·
分子生物学
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PubMed
高影响因子
危险品化学品经营许可证（带存储）