JOURNAL OF ANALYTICAL TOXICOLOGY
·
2015
·Vol. 39
·期 7
·551-556
·
IF 2.858
Wang Ting,Yu Zhiguo,Shi Yan,Xiang Ping
At the global level, seizures of crystalline methamphetamine (MA) and MA tablets have risen to a new high, indicating that the substance is an imminent threat. MA enantiomer profiling was a useful tool to investigate the prevalence of MA abuse, the intrinsic characteristics of the seized samples and the trends of precursors. In this work, the distribution of enantiomers in clandestine MA crystals and tablets seized mainly in the Yangtze River Delta region, China, from 2008 to 2014 were identified. The MA samples were diluted with internal standard methanol solution, and analyzed by LC–MS-MS. The detection limits of the enantiomers were 0.04 μg/L. The limit of quantification was 0.1 μg/L. As little as 0.2% of the R-enantiomer ratio could be determined. Standard calibration curves of S- and R-MA showed good linearity in the range of 0.1–80 μg/L (r2 > 0.995). All of the seizures were optically pure S-enantiomer in the years 2008 and 2009. Seized samples containing a slight amount of R-MA began to appear in 2010 and increased in the year 2014. No racemic mixture or R-isomer of MA was seized. From this study, we could find out that smuggling routes and/or precursors might be silently changing in the Yangtze River Delta region, China.
研究领域:
分析化学
·
法医学
·
药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2022
·Vol. 45
·期 18
·3431-3442
·
IF 3.614
Zhe Chen,Guangli Yan,Yu Yang,Hui Sun,Aihua Zhang,Ying Han,Shugui Wang,Xijun Wang
Naoling Pian is a prescription composed of 15 herbs, which is mainly used for the treatment of insomnia in clinical practice. However, the chemical constituents in Naoling Pian are numerous and unclear, which hinders the interpretation of its bioactive constituents and the subsequent research on the material basis for pharmacodynamics. The purpose of this study is to develop a rapid method for identifying the chemical constituents of Naoling Pian using high-throughput ultra-performance liquid chromatography quadrupole time of flight coupled with mass spectrometry combined with a software platform for data processing. The whole composition of Naoling Pian was characterized in positive and negative ion modes. In this experiment, an overall total of 201 constituents were identified by using reference standards, online and self-built databases matching, fragmentation rules analysis of mass spectrometry peaks with a software platform. Meanwhile, Naoling Pian was analyzed for the first time using liquid chromatography–mass spectrometry method, the constituents could be identified in a quick and accurate manner, and the results could provide a scientific basis for the follow-up research on the pharmacodynamic material basis and quality control of Naoling Pian.
研究领域:
药理学
·
分析化学
·
中医药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Environmental Science-Water Research & Technology
·
2023
·Vol. 9
·期 4
·1231-1237
·
IF 5
Run Zhou,Zhifei Xu,Yukang Wu,Li Yang,Xiuzhu Li,Yuanhua Meng,Pengfei Zhu,Lingcan Kong,Xinliang Ding
Human exposure to disinfection by-products (DBPs) primarily occurs through the consumption of drinking water. Haloacetamides (HAcAms) are an emerging class of nitrogenous DBPs with higher levels of cytotoxicity and genotoxicity compared to those of regulated DBPs. Detecting ultra-trace levels of HAcAms in drinking water remains challenging despite the availability of multiple detection methods. This paper reports the first use of ultra-performance liquid chromatography–mass spectrometry/mass spectrometry (UPLC-MS/MS) to quantify 13 HAcAms in drinking water without pretreatment. Results from the analysis of water samples collected from four cities in East China showed total HAcAm concentrations of 0.21–6.12 μg L−1, which were comparable to previously reported data from other countries. Further, 11 out of 13 HAcAms were detected in 60 water samples, with diHAcAms being the predominant subclass. DCAcAm and BCAcAm were the primary HAcAms targeted for detection and two Iodo-HAcAms were detected. The average total HAcAm concentration in water samples disinfected with chloramine was significantly higher than that in water samples disinfected with chlorine. Additionally, the total HAcAm concentrations in water samples from a treatment plant (WTP) using the ozone-biological activated carbon (ozone-BAC) process were lower than those in water samples from WTPs that did not use this treatment process. The results of this study have significant implications for monitoring water quality and protecting human health.
研究领域:
环境科学
·
公共卫生
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2023
·Vol. 37
·期 4
·e5584
·
IF 1.8
Kaiyue Ren,Yanjuan Yuan,Qing Shao,Hongqun Qiao
For the further study of [ 19 F] - alfatide, the development of highly sensitive analytical methods for its determination is an urgent issue. In this paper, a method for simultaneously determining [ 19 F]-alfatide and alfatide using liquid chromatography/tandem mass spectrometry was created and validated. The plasma samples were pretreated using the protein precipitation method. Poroshell 120 EC-C 18 (4.6 × 50 mm, 2.7 μm, Agilent) was used for the separation of the analytes to be measured. The mobile phase, consisting of acetonitrile and water (0.1% acetic acid, 50:50, v/v), was delivered at a flow rate of 0.60 ml/min for sample analysis. Positive electrospray ionization was performed using multiple-reaction monitoring with transitions of m / z 715.2 → 636.6 for [ 19 F]-alfatide, the ion pairs 700.3 → 851.5 for alfatide and the ion pairs 237.1 → 194.2 for carbamazepine (internal standard). According to the results, the method had high specificity, precision and accuracy as well as an extended linear range. The matrix effect and extraction recovery were also acceptable. The method was successfully applied to the pharmacokinetic study of [ 19 F]-alfatide in rats.
研究领域:
分析化学
·
药理学
·
药物代谢
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF LIPID RESEARCH
·
2022
·Vol. 63
·期 12
·
IF 6.676
Xian Fu,Hou-Hua Yin,Ming-Jun Wu,Xin He,Qing Jiang,Ling-Tong Zhang,Jun-Yan Liu
Oxylipins are important biological regulators that have received extensive research attention. Due to the extremely low concentrations, large concentration variations, and high structural similarity of many oxylipins, the quantitative analysis of oxylipins in biological samples is always a great challenge. Here, we developed a liquid chromatography-tandem mass spectrometry-based method with high sensitivity, wide linearity, and acceptable resolution for quantitative profiling of oxylipins in multiple biological samples. A total of 104 oxylipins, some with a high risk of detection crosstalk, were well separated on a 150 mm column over 20 min. The method showed high sensitivity with lower limits of quantitation for 87 oxylipins, reaching 0.05–0.5 pg. Unexpectedly, we found that the linear range for 16, 18, and 17 oxylipins reached 10,000, 20,000, and 40,000 folds, respectively. Due to the high sensitivity, while reducing sample consumption to below half the volume of previous methods, 74, 78, and 59 low-abundance oxylipins, among which some were difficult to detect like lipoxins and resolvins, were well quantified in the tested mouse plasma, mouse liver, and human plasma samples, respectively. Additionally, we determined that analytes with multifarious concentrations of over a 1,000-fold difference could be well quantified simultaneously due to the wide linearity. In conclusion, most likely due to the instrumental advancement, this method effectively improves the quantitative sensitivity and linear range over existing methods, which will facilitate and advance the study of the physiological and pathophysiological functions of oxylipins.
研究领域:
分析化学
·
生物化学
·
药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Frontiers in Pharmacology
·
2023
·
IF 5.6
Jirui Lang,Li Li,Yunyun Quan,Ruirong Tan,Jinbiao Zhao,Min Li,Jin Zeng,Shilong Chen,Ting Wang,Yong Li,Junning Zhao,Zhujun Yin
Wuwei Shexiang Pill (WSP) is a Tibetan traditional medicine, which has been demonstrated to exhibit potent anti-inflammatory and anti-gout effects. However, the specific pharmacological mechanism is not elucidated clearly. In the present study, liquid chromatography-mass spectrometry (LC-MS)-based metabolomics was applied to investigate the alteration of serum metabolites induced by WSP treatment in MSU-induced gouty rats. Subsequently, bioinformatics was utilized to analyze the potential metabolic pathway of the anti-gout effect of WSP. The pharmacodynamic data discovered that WSP could ameliorate ankle swelling and inflammatory cell infiltration, as well as downregulate the protein expression of IL-1β, p-NF-κB p65, and NLRP3 in the synovial membrane and surrounding tissues of gouty ankles. LC-MS-based metabolomics revealed that there were 30 differential metabolites in the serum between sham-operated rats and gouty ones, which were mainly involved in the metabolism of fructose and mannose, primary bile acid biosynthesis, and cholesterol metabolism. However, compared to the model group, WSP treatment upregulated 11 metabolic biomarkers and downregulated 31 biomarkers in the serum. KEGG enrichment analysis found that 27 metabolic pathways contributed to the therapeutic action of WSP, including linoleic acid metabolism, phenylalanine metabolism, and pantothenate and CoA biosynthesis. The comprehensive analysis-combined network pharmacology and metabolomics further revealed that the regulatory network of WSP against gout might be attributed to 11 metabolites, 7 metabolic pathways, 39 targets, and 49 active ingredients of WSP. In conclusion, WSP could ameliorate the inflammation of the ankle in MSU-induced gouty rats, and its anti-gout mechanism might be relevant to the modulation of multiple metabolic pathways, such as linoleic acid metabolism, phenylalanine metabolism, and pantothenate and CoA biosynthesis. This study provided data support for the secondary development of Chinese traditional patent medicine.
研究领域:
药理学
·
代谢组学
·
传统中药
·
炎症生物学
·
生物信息学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2016
·Vol. 55
·期 1
·60-68
·
IF 1.32
Gu Liqiang,Shi Huiyan,Zhang Ruowen,Wei Zhe,Bi Kai-Shun,Chen Xiao-Hui
In clinical diagnosis, serum creatinine (CR) was commonly used as the routine markers for the evaluation of kidney injury. To investigate the specific and sensitive nephrotoxicity biomarkers in different drug-induced kidney injury (DKI) models, receiver operating characteristic (ROC) analysis was applied in this study. The quantification data were acquired by the LC–MS determination. Histopathology results showed that different kinds of kidney injuries were observed in different DKI models (gentamycin, cisplatin, methotrexate and amphotericin B models), indicating the injuries might be caused by different mechanisms. Then, five typical biomarkers were simultaneously determined by a newly developed and validated LC–MS method. Uric acid, CR, hippuric acid, 3-indoxyl sulfate and phenaceturic acid were separated by an Apollo C18 column and a methanol/water (5 mM ammonium acetate) gradient program. The prepared calibration curves showed good linearity with regression coefficients all above 0.9927. Of all the analytes, the precision were below 9.9% and the accuracy were from −10.3% to 9.2%. ROC results showed that different nephrotoxicity biomarkers were specific in different DKI models. The changes of different biomarkers might be induced by different nephrotoxic mechanisms in the DKI models. These specific and sensitive biomarkers in combination with serum CR are promising in the clinical diagnosis of DKI.
研究领域:
毒理学
·
临床医学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Antioxidants
·
2019
·Vol. 8
·期 8
·321
·
IF 4.52
Dandan Wang,Liangxiao Zhang,Yueqing Xu,Xin Qi,Xuefang Wang,Xiupin Wang,Qi Zhang,Peiwu Li
Sesame is a nutritional agricultural product with medicinal properties. Accurate determination of micronutrients is important for the improvement of sesame quality and nutrition assessments. Our previous study showed that 10 antioxidants—d-homoproline, vitamin B2, coniferyl aldehyde, hesperidin, phloretin, N-acetyl-l-leucine,l-hyoscyamine, ferulic acid, 5-methoxypsoralen, and 8-methoxypsoralen—in sesame were potential characteristic nutrients in sesame. Herein, simultaneous detection of 10 different types of antioxidants was developed by using ultrasound-assisted extraction coupled with liquid chromatography-tandem mass spectrometry (UAE-LC-MS/MS) with the help of response surface methodology. The significant variables and levels were screened and optimized by combining the single factor experiment, Plackett–Burman test, and Box–Behnken design. The optimal conditions for extraction of target antioxidants in sesame were methanol solution of 75.0%, liquid-to-material ratio of 20:1 (mL/g), extraction temperature of 50 °C, extraction power of 410.0 W, extraction time of 65 min. The total yield of targets was 21.74 μg/g under the optimized conditions. The mobile phase used was 0.1% formic acid in acetonitrile and 0.1% formic acid in water, and the column was a Thermo Syncronis C18 reverse phase column (100 mm × 2.1 mm, 3 μm). All targets required only one injection and could be quickly separated and assayed within 7 min. The limits of detection and limits of quantification for these 10 nutritional compounds ranged from 0.01 to 0.11 µg/kg and from 0.04 to 0.34 µg/kg, respectively. The validation results indicated that the method had reasonable linearity (R2≥ 0.9990), good recoveries (71.1%–118.3%), satisfactory intra-day precision (≤9.6%) and inter-day precision (≤12.9%), and negligible matrix effects (≤13.8%). This simultaneous quantification method was accurate, fast, and robust for the assessment of sesame nutrition.Keywords:antioxidants;ultrasound-assisted extraction;liquid chromatography-tandem mass spectrometry (LC-MS/MS);sesame;simultaneous detection;response surface methodology
研究领域:
食品科学
·
分析化学
·
营养学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
PHYTOMEDICINE
·
2023
·
IF 7.9
Jingya Ruan,Huimin Li,Mengqi Lu,Mimi Hao,Fan Sun,Haiyang Yu,Yi Zhang,Tao Wang
Background Jujube, a popular fruit from the Rhamnaceae family, relieves colorectal inflammation caused by spleen deficiency and has been used in many formulas in clinical for decades to treat colorectal cancer (CRC). As of yet, the therapeutic substances and mechanism of their action are unknown. Purpose The purpose of this study is to define the therapeutic substances of jujube and its mechanism of action in treating CRC . Methods The pharmacological effects of jujube extract and its fractions were evaluated in vivo using a CRC mouse model induced by AOM/DSS. The DAI value, colon length, mortality, tumor burden, and histological tumor size of the treated animals were compared. To explore the potential therapeutic substances, LC-MS analysis was conducted to characterize the serum migration components. A network pharmacology experiment was carried out for potential molecular targets. To verify the therapeutic substances as well as the molecular mechanism of jujube intervening CRC, cellular MTT assay of the serum migration components, Western blot and IHC tests were conducted. Results The in vivo pharmacological studies showed that compared to AOM/DSS treated mice, the mortality and DAI value, tumor burden, and histological tumor size of jujube extract and its fat-soluble fraction (mainly contained triterpenes) treated mice were significantly reduced, and their colon lengths were obviously longer than AOM/DSS treated mice. The targeted-LC/MS analysis supposed triterpenes 3, 7, 9, 11, 12, 14, 17 – 21, and 25 – 28 to be the serum migration components, which might be the potential therapeutic substances. In the network pharmacology experiment, the GO annotation and enrichment analysis of the KEGG pathway indicated that PI3K-Akt pathway and inflammatory reaction were important factors for jujube inhibiting CRC. Cellular MTT assay of serum migration components indicated that the potential effective substances from fat-soluble fraction to be triterpenes 3, 7, 17, 19, 20, and 25. The Western blot and IHC assays implied that the jujube extract, its fat-soluble fraction, and triterpenes 7, 17, and 20 showed inhibition on the expression of PI3K/Akt/NF-κB signaling pathway-related proteins. Additionally, it was noted in the pharmacodynamic experiment that ZJL's effectiveness was more apparent than ZJH and SQL in tumor burden rate, colon length, and spleen weight, which indicated that the efficacy of ZJ is contributed from CD and SQ, and they may have a synergistic effect on anti-CRC. Conclusion These results for the first time provide evidence that jujube triterpenes possess an anti-CRC effect, their mechanism was involving the control of the PI3K/Akt/NF-κB signaling pathway. What's more, the potential synergistic effect of the fat-soluble and water-soluble components found in this study provided a solid foundation for our deep understanding of how jujube can ameliorate CRC.
研究领域:
药理学
·
肿瘤学
·
分子生物学
·
中医药
✓ 已验证
产品关联
DOI
PubMed
高影响因子
DRUG METABOLISM AND DISPOSITION
·
2025
·
IF 4
Yixuan Wang,Tingting Yu,Xinjie Zhang,Yutong Wang,Lanlan Gui,Wushuang Zeng,Liang Huang,Ke Lan
Sterol 12α-hydroxylase (CYP8B1) is a key regulator of bile acid (BA) homeostasis and an emerging therapeutic target for metabolic disorders. To address the challenge of cellular CYP8B1 inhibition characterization, this work developed a pharmacologically optimized HepG2 cells model using triiodothyronine-dexamethasone-bezafibrate (TDB) induction, which significantly enhances the 12α-hydroxylation activity along the acidic pathway of BA biosynthesis in HepG2 cells. Employing stable isotope tracing with apolipoprotein A1-solubilized 2,3,4- 13 C 3 -cholesterol, we established an LC-MS-based flux analysis platform to track de novo BA synthesis. Combined with recombinant CYP8B1 assay, flux analysis revealed CYP8B1 participates in cholic acid synthesis in HepG2 cells, typically via 12α-hydroxylation of 7α-hydroxy-3-oxo-4-cholestenoic acid and dihydroxycholestanoic acid. In TDB-HepG2 cells, azole antifungals exhibited differentiated inhibition of 12α-hydroxylation activity, generally mirroring the enzymatic data. Econazole acted as a relatively selective CYP8B1 inhibitor with cellular half maximal inhibitory concentration of 0.31-0.45 μM, tioconazole and posaconazole dually inhibited CYP8B1 and sterol 27-hydroxylase (CYP27A1), itraconazole and voriconazole primarily inhibited CYP27A1, and fluconazole showed no activity toward either enzyme. This study provides the first direct evidence that CYP8B1 participates in cholic acid synthesis via acidic pathway and establishes a high-throughput cellular platform for screening CYP8B1 inhibitors, revealing azoles as effective modulators of this pathway.
研究领域:
分子生物学
·
药物代谢
·
肝脏病学
·
代谢组学
·
生物化学
·
药理学
·
细胞生物学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
WATER RESEARCH
·
2024
·
IF 11.4
DongMing Cai,Jinjian Ding,Fangfang Li,Guoqiang Zhuang,Minjie Li,Liang-Hong Guo
Many antibiotic disinfection byproducts have been detected but their toxicity has not been evaluated adequately. In this report, the chlorination reaction kinetics of five common sulfamides (SAs), reaction intermediates and their toxicity were investigated. Chlorination of sulfapyridine (SPD), sulfamethazine (SMT), sulfathiazole (STZ), and sulfisoxazole (SIZ) followed the second-order kinetics, and were degraded completely within 10 min. A large number of reaction intermediates were deteced by LC-MS, among which a total of 16 intermediates were detected for the first time. Toxicity of the five SAs chlorination solutions was evaluated separately by examining their effects on the growth rate of S. salivarius K12 , a commensal bacterium in the human digestive system. After 30 min chlorination, solutions of SMT, STZ and sulfadiazine (SDZ) each exhibited severe toxicity by inhibiting the bacteria growth completely, whereas the inhibition was only 50 % and 20 % by SIZ and SPD respectively. Based on the comparison between toxicity test results and mass spectra, three SA chlorination intermediates, m/z 187.2 (C 10 H 10 N 4 ), m/z 287.2 (C 9 H 7 N 3 O 4 S 2 ) and m/z 215 (C 7 H 10 N 4 O 2 S/C 12 H 14 N 4 ) were proposed to be the primary toxicants in the chlorination products. Our study demonstrated the power of combined approach of chemical analysis and toxicity testing in identifying toxic disinfection byproducts, and highlighted the ne ed for more research on the toxicity evaluation and risk assessment of antibiotic disinfection byproducts.
研究领域:
环境化学
·
毒理学
·
微生物学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Frontiers in Chemistry
·
2022
·
IF 5.545
Jiang Zhehui,Wang Tianhao,Zhang Kaixue,Zhang Meiqi,Ma Ling,Ren Weichao,Bao Yihong,Ma Wei
Light quality consists of a spectrum of different bands, which not only affects plant, development, and primary metabolism but also affects the secondary metabolism of plants. It is an important factor affecting the content of active components of medicinal plants. The A. paniculata seedlings planted in the laboratory, as materials, were tested with red light, far red light, blue light, and ultraviolet light separately. The study assays the content of six main chemical components separately by LC-MS, observes the changes in the content, and analyzes the relationship between the light quality and the active ingredient of A. paniculata. Using the ointment yield and pH value, the fingerprint analysis method of A. paniculata standard decoction was established, and we discussed the selection of index components of A. paniculata standard decoction. It was suggested to select andrographolide as the index component. It will provide a theoretical basis for the large area cultivation of A. paniculata and optimize the quality of medicinal materials to ensure the quality of standard decoction.
研究领域:
生药学
·
植物生理学
·
药物化学
✓ 已验证
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）