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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2015 · IF 2.912

Fast and Online Determination of Five Avermectin Residues in Foodstuffs of Plant and Animal Origin Using Reusable Polymeric Monolithic Extractor Coupled with LC-MS/MS

Xin Li,Man-Man Wang,Guo-Ying Zheng,Lian-Feng Ai,Xue-Sheng Wang

A hydrophobic monolith (10 mm × 2.1 mm i.d.) was developed as a reusable online solid-phase extraction (SPE) sorbent coupled with LC-MS/MS for the rapid determination of five avermectin residues in foodstuffs of both plant and animal origin. The online SPE was achieved using a 10 mmol/L ammonium acetate solution as the loading solvent, and acetonitrile (MeCN) was selected for the washing step. After being transferred from the monolith into a C18 analytical column using MeCN, the analytes were analyzed by LC-MS/MS using MeCN/0.1% NH4OH (10:90, v/v) as the mobile phase. The detection limit was 2 μg/kg for five avermectins, and the recoveries in fresh pear, chili seed, bovine muscle, and milk ranged from 71.8% to 101.3% with relative standard deviations of less than 8.94%. The online SPE and determination were achieved within 15 min, and the monolithic extractor was reusable for more than 500 experiments.

CAS / MDL: 97-88-1
研究领域: 分析化学 · 食品安全
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF NUTRITIONAL BIOCHEMISTRY · 2024 · IF 4.8

Lipidomic profiling of serum and liver tissue reveals hepatoprotective mechanism of taxifolin in rats with CCl4-induced subacute hepatic injury based on LC-MS/MS

Yiming Ni,Xinghua Chen,Yiqun Jia,Long Chen,Mingmei Zhou

Currently, the hepatoprotective activity of taxifolin, a flavonoid isolated from Pseudotsuga taxifolia , has been reported in many animal models. However, whether the protective effect of taxifolin on the liver is related to its effect on lipidomics is unclear. Based on the significant therapeutic effect of taxifolin on CCl 4 induced subacute hepatic injury, we observed the intervention of taxifolin by lipidomics. The results demonstrate that taxifolin can effectively reverse the damage caused by CCl 4 , which including hepatocyte vacuolization and necrosis. Lipomic profiling based on liquid chromatography-mass spectrometry showed that taxifolin was able to restore lipidomic changes caused by CCl 4 , including the levels of lysophosphatidylserine (LPS), phosphatidylcholine (PC), coenzyme (Co), phosphatidylglyceride (PG), phosphatidylserine (PS), dimethylphosphatidylethanolamine (dMePE), ceramide (Cer), sphingosine (So), triglycerides (TG), and monogalactosyl diacylglycerol (MGDG) in the rat liver, and phosphatidylcarbinol (PMe) and phosphatidylethanolamine (PE), plant sphingosine (phSM), glucose ceramide (CerG1), TG, and diglycerides (DG) in serum. Spearman's correlation analysis showed that CerG1, phSM, PE, and PMe in serum, and Cer, dMePE, PG, PS, So, TG, and MGDG in liver were positively correlated with serum levels of aspartate transaminase, alanine transaminase, and liver index; while TG, DG in serum, and Co, LPS, PC in liver were negatively correlated with the parameters. In total, 43 and 34 lipid molecules were altered by taxifolin treatment in the liver and serum, respectively, mainly including glycerophosphoglycerols, glycerophosphocholines, glycerophosphoethanolamines, and linoleic acids and derivatives. Our findings help to provide novel insights into the mechanism of the hepatoprotective effect of taxifolin from a lipidomics approach.

CAS / MDL: 56-23-5
研究领域: 药理学 · 代谢组学 · 肝脏病学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Analytical Methods · 2024 · IF 2.7

Characterisation of the phytochemical and bioactivity profiles of raw tea, stale-aroma, and betelnut-aroma type of Liupao tea through GC/LC-MS-based metabolomics

Xuancheng Wang,Zhiyong She,Hailin Zhou,Tingting An,Jianwen Teng,Ning Xia,Pingchuan Zhu,Wenhui Liu,Huanxiao Dong,Limin Tang,Shulan You,Lu Wei,Kongying Li,Lingli Wang,Li Huang,Qisong Zhang

Liupao tea (LPT) is a Chinese dark tea known to possess a unique flavour. Microbial fermentation plays a crucial role in flavour development and enrichment. Currently, the phytochemical profiles and bioactivities of LPT with and without fermentation are not fully known. In this study, we compared the chemical composition of raw tea (SF), stale-aroma (SA), and betelnut-aroma (BA) type LPT through the application of GC/LC-MS-based metabolomics, and experimentally investigated their bioactivities via antioxidant, anti-inflammatory, hypolipidemic, and hypoglycemic assays in vitro. The results indicated that fermentation enhanced the flavour of LPT as evidenced by the sweetness-producing substances, decreased bitterness and astringency-related compounds and enriched abundance of aroma-generating compounds. Two and four volatiles were detected to be major contributors to the aroma in SA and BA, respectively. Fatty acids and phosphatidylcholines were the primary lipids, among which the lysing diacylglycerol trimethyl homoserines were found to be a new class of lipids in LPT. Notably, the fermentation resulted in the degradation of compounds, particularly glycerophospholipids and saccharolipids. SF had the highest level of bioactivity, followed by BA and SA. These findings expand the present understanding regarding the development of flavour, nutrition, and medicinal value of LPT. Moreover, they provide a theoretical basis for the identification of BA and SA and serve as a reference value for consumers in their selection of LPT products.

CAS / MDL: 1898-66-4 28752-68-3
研究领域: 食品科学 · 药理学 · 代谢组学 · 茶叶科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD RESEARCH INTERNATIONAL · 2023 · IF 8.1

Impact of storage time on non-volatile metabolites and fungal communities in Liupao tea using LC-MS based non-targeted metabolomics and high-throughput sequencing

Yingyi Huang,Huahong Liu,Xiaohua Zhang,Yuxin Wu,Zhusheng Liu,Yuelan Pang,Renjun Liu,Chun Yang,Jinfang Nie

Long-term storage of Liupao tea (LPT) is usually believed to enhance its quality and commercial value. The non-volatile metabolites variations and the fungal succession play a key role for organoleptic qualities during the storage procedure. To gain in-depth understanding the impact of storage time on the quality of LPT, two different brands of LPT with different storage time, including Maosheng LPTs (MS) with 0, 5, 10 and 15 years and Tianyu LPTs (TY) with 0, 3, 5, 8 and 10 years, were resorted to investigate the changes of non-volatile metabolites and fungi as well as their correlation by multi-omics. A total of 154 and 119 differential metabolites were identified in these two different brands of MS and TY, respectively, with the aid of high-performance liquid chromatography with quadrupole-time-of-flight mass spectrometry. In both categories of LPTs, the transformation of differential metabolites in the various stages referred to the formation of alkaloids, increase of organic acids, biosynthesis of terpenoids as well as glycosylation and methylation of flavonoids. Thereinto, glycosylation and methylation of flavonoids were the critical stages for distinguishing MS and TY, which were discovered in MS and TY stored for about 10 and 8 years, respectively. Moreover, the results of high-throughput sequencing showed that the key fungal genera in the storage of LPTs consisted of Eurotium , Aspergillus , Blastobotrys , Talaromyces , Thermomyces and Trichomonascus . It was confirmed on the basis of multivariate analysis that the specific fungal genera promoted the transformation of metabolites, affecting the tea quality to some extent. Therefore, this study provided a theoretical basis for the process optimization of LPT storage.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2020 · IF 3.209

Pharmacovigilance of herb-drug interactions: A pharmacokinetic study on the combination administration of herbal Kang’ai injection and chemotherapy irinotecan hydrochloride injection by LC–MS/MS

Yanfei Chen,Zhaoliang Hu,Wenzhu Qi,Shuxiao Gao,Jing Jiang,Shixiao Wang,Lei Xu,Xin Xu,Min Song,Taijun Hang

Chinese herbal drugs are often combined with chemotherapy drugs for the treatment of cancers. However, the combination administrations often do not have scientifically sound bases established on full preclinical and clinical investigations. A commonly used anti-colon-cancer herb-drug pair, irinotecan (CPT-11) hydrochloride injection and Kang’ai (KA) injection was taken as an example to investigate the possible pharmacokinetic interactions between Chinese herbal drugs and chemotherapy injections to determine the potential adverse drug reactions (ADRs). Rats were randomly divided into three groups and received 20 mg/kg CPT-11 injection 15 min after administration of 4 mL/kg saline for the CPT-11 single administration group and 4 mL/kg KA injection for the separated co-administration group, respectively. In the pre-mixed co-administration group, rats received a mixture of 20 mg/kg CPT-11 injection and 4 mL/kg KA injection. Blood samples were collected at 10 pre-determined time points between 0 and 24 h. The tissue samples were collected at 5 and 8 min after the injections, respectively. A reliable LC–MS/MS method was established for the simultaneous determination of CPT-11 and its metabolites, SN-38, SN-38 G and APC in the rat plasma and tissue samples, after full confirmation of two injections chemical and stability compatibilities. Compared to the C 0 (5129 ± 757 ng/mL) and AUC 0-t (7858 ± 1307 ng h/mL) of CPT-11 in the CPT-11 single administration group, the C 0 (4574 ± 371 ng/mL) and AUC 0-t (8779 ± 601 ng h/mL) after the separated co-administration remained unchanged, but the pre-mixed co-administration resulted with a significant increased C 0 (29,454 ± 12,080 ng/mL) and AUC 0-t (15,539 ± 5165 ng h/mL) (p < 0.05). Since the exposures of CPT-11 in most tissues in the pre-mixed co-administration group were dramatically lower than the separated co-administration group, the increased CPT-11 plasma concentration may be produced by the delayed tissue distribution because of the encapsulation by the components contained in KA injection, such as polysaccharides. Similar differences were also found in its metabolite, SN-38 G. There are obvious herb-drug interactions between CPT-11 injection and KA injection after the pre-mixed co-administration. The resulting excessive CPT-11 in the plasma may lead to many serious ADRs. Therefore, the full evaluation of herb-drug interactions is necessary and inappropriate combinations should be avoided.

CAS / MDL: 7689-03-4 86639-52-3
✓ 已验证 产品关联 DOI PubMed 高影响因子
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PREPARATIVE BIOCHEMISTRY & BIOTECHNOLOGY · 2019 · IF 1.117

Preparation of hepatic stimulator substance from neonatal porcine liver by enzymatic hydrolysis and characterization of the liver proteins by LC-MS/MS bottom-up approach

Leilei Zhao,Qiong Jiang,Sitong Luo,Jie Shen,Xinjun Xu

Hepatic stimulator substance (HSS) is prepared by the freeze–thaw method on a large scale, but it is time-consuming and inefficient. It is necessary to find a better method to improve the efficiency and yield of HSS. In this study, HSS was prepared by enzymatic hydrolysis of neonatal porcine liver with trypsin, papain, dispase, and alcalase. Relatively, dispase was found to be the best enzyme, based on the results of the degree of hydrolysis and MTT assay. Box–Behnken design-response surface method was used to optimize the conditions, which were as follows: enzyme (dispase) concentration, 4164 U/g; substrate concentration, 7% (w/v); hydrolysis time, 4.3 hr; temperature, 45 °C; and pH, 6.5. The degree of hydrolysis was (54.99 ± 1.57)%. Shotgun proteomics coupled with Gene Ontology (GO) analysis based on the PANTHER classification system was used to screen proteins from neonatal porcine liver. The results profiled the proteins into biological processes, molecular functions, and cellular components, thus laying a foundation for further studies on components involved in and mechanisms of liver regeneration. Overall, the results suggest that enzymatic hydrolysis might be a promising method for industrial application.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2019 · IF 2.983

Development of an underivatized LC-MS/MS method for quantitation of 14 neurotransmitters in rat hippocampus, plasma and urine: Application to CUMS induced depression rats

Xue-Mei Han,Yan-Jie Qin,Ying Zhu,Xin-Lin Zhang,Nan-Xi Wang,Ying Rang,Xue-Jia Zhai,Yong-Ning Lu

Sensitive and comprehensive measurement of systemic metabolites of tryptophan, phenylalanine and glutamate metabolism in biological samples is effective for understanding the pathogenesis of depression and other neurological diseases. Therefore, this study developed an underivatized liquid chromatography tandem mass spectrometry (LC–MS/MS) method for simultaneous monitoring the 3 components of glutamate metabolism in rat hippocampus and 11 components of tryptophan and phenylalanine metabolism in rat hippocampus, plasma and urine, and applied it to investigate their changes in rats induced by chronic unpredictable mild stress (CUMS). The investigated analytes are as follows: tryptophan, serotonin, 5-hydroxyindoleacetic acid, kynurenine, kynurenic acid, xanthurenic acid, 3-hydroxyanthranilic acid, quinolinic acid, phenylalanine, tyrosine, tyramine, glutamate, glutamine and gamma-aminobutyric acid. The method was verified to be sensitive and effective with satisfactory linearity, accuracies in the range of 78.2%–120.4%, and precisions less than 17.8% for all identified analytes. A series of significant changes in CUMS-induced rats can be detected: tryptophan, serotonin and tyrosine levels decreased and quinolinic acid increased in both hippocampus and plasma. In addition, the kynurenine/tryptophan ratios increased in hippocampus and plasma, the kynurenic acid/quinolinic acid ratios of plasma and urine were significantly reduced. These findings demonstrated that the CUMS procedure could lead to the central and peripheral imbalances of tryptophan and phenylalanine metabolism. In conclusion, a LC–MS/MS method for simultaneous measurement of several neurotransmitters in rat hippocampus, plasma and urine was developed and successfully applied to investigation of the central and peripheral changes in CUMS-induced rats. The method would be expected to provide applicability to the study of the mechanisms of depression and other related diseases associated with these neurotransmitters.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF SEPARATION SCIENCE · 2019 ·Vol. 43 ·期 3 ·590-597 · IF 2.516

Simultaneous quantification of atractyloside and carboxyatractyloside in rat plasma by LC-MS/MS: Application to a pharmacokinetic study after oral administration of Xanthii Fructus extract

Hong Pan,Feng Yang,Daiyuan Xiang,Fuguo Shi

Xanthii Fructus is extensively used as an herbal medicine. Ingestion of this herb is associated with severe hepatotoxicity and nephrotoxicity. Atractyloside and carboxyatractyloside are two dominative toxic constituents in Xanthii Fructus. However, their pharmacokinetic study is lacking. In this study, a novel high-performance liquid chromatography-tandem mass spectrometry method was developed to simultaneously quantify the rat plasma concentrations of atractyloside and carboxyatractyloside. After protein precipitation, the analytes were chromatographic separated on a ZORBAX Eclipse Plus column (2.1 × 150 mm id, 5 µm) under gradient elute. In the negative electrospray ionization mode, the transitions at m/z 725.3→645.4 for atractyloside, m/z 769.3→689.4 for carboxyatractyloside, and m/z 479.2→121.1 for paeoniflorin (the internal standard) were acquired by multiple reaction monitoring. This analytical method showed good linearity over 1–500 ng/mL for atractyloside and 2–500 ng/mL for carboxyatractyloside with acceptable precision and accuracy. No matrix effect, instability and carryover occurred in the analysis procedure. The extraction recoveries were greater than 85.0%. This method was applied to a preliminary pharmacokinetic study by orally administering Xanthii Fructus extract (9 g/kg) to rats, which was useful to evaluate the role of these two compounds in Xanthii Fructus-induced toxicity.

CAS / MDL: 631-61-8
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2017 · IF 3.255

Development of a LC–MS/MS method to investigate the interference of pharmacokinetics of the main constituents in Saxifraga stolonifera: Involvement of drug metabolism enzymes

Yuan Wang,Qing Li,Yue Dai,Ronghua Pan,Yufeng Xia

A specific and sensitive LC–MS/MS method was established for the simultaneous determination of bergenin, protocatechuic acid and gallic acid, the main active constituents of Saxifraga stolonifera (L.) Meerb. herb, in rat plasma. After fully validated, the method was applied to the comparative pharmacokinetic studies of the three compounds orally administered alone and in combination in the S. stolonifera extract, respectively. The results showed that the pharmacokinetic parameters, including C max , T max , AUC, CL z /F, MRT 0-∞ , were significantly different for both bergenin and protocatechuic acid in the extract as compared to the corresponding compounds administered alone. However, the pharmacokinetic behavior of gallic acid in the extract did not differ from that administered alone. Further studies found that quercetin, coexisting in the herb extract, significantly decreased the glucuronidation of bergenin through inhibiting the activities of UGT1A1 and UGT1A3, and reduced the metabolism of protocatechuic acid by inhibiting the activity of catechol-O-methyltransferase. Quercetin and other flavonoids occurring in the S. stolonifera extract might increase the absorption and improve the bioavailability of bergenin and protocatechuic acid by slowing down the liver metabolism. The findings provide a good guidance for the development and clinical application of S. stolonifera .

✓ 已验证 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY A · 2025 · IF 4

Development of a procedure based on dispersive solid phase extraction and LC-MS/MS for the analysis of perfluoroalkyl and polyfluoroalkyl substances in food contact materials

Yang Yang,Jin Wang,Jia Qiu,Yan Luo,Chun Yang,Shali Tang,Hui Cao,Qian Wang,Xiaojing Lai

To monitor per- and polyfluoroalkyl substances (PFAS) in food contact materials (FCMs), an LC-MS/MS method for the simultaneous detection of 35 PFAS was developed and validated in paper and plastic products. Chromatographic and mass spectrometry parameters, extraction solvents, matrix effects in details were studied. The impact of matrix effects on PFAS concentration was analyzed, revealing that the matrix enhancement effect was more significant for some PFAS with low concentrations. In order to eliminate the matrix effect and enhance detection accuracy, a straightforward pretreatment method combining methanol ultrasonic extraction with dispersive solid-phase extraction (d-SPE) was established. PFHpA, PFDA, PFTriDA, PFTeDA, PF-3,7-DMOA, HFPO-DA, PFHxS, PFHpS, PFOS, 4:2 FTS, 6:2 FTS, 8:2 FTS, 10:2 FTS, and 6:2 diPAP required further d-SPE extraction with PSA, and other substances could be directly extracted by methanol ultrasonic treatment. The recoveries of the established method for all compounds ranged from 62.40 to 135.80%, with a relative standard deviation (RSD) of 0.15% to 16.81%. The limit of quantitation was between 0.005 and 0.02 mg·kg −1 . The method was applied to detect PFAS in 119 FCMs, resulting in the identification of 15 PFAS.

CAS / MDL: 64-18-6
研究领域: 分析化学 · 食品安全
✓ 已验证 产品关联 DOI PubMed 高影响因子
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2025 · IF 3.8

Development and validation of an isotope dilution-liquid chromatography (ID-LC–MS/MS)-based candidate reference measurement procedure for total 3,3′,5-triiodothyronine in human serum

Li Wenya,Gao Bingling,Yang Tao,Tang Liping,Song Dan,Li Hongmei,Sun Keqi,Xiao Peng

3,3′,5-Triiodothyronine (T3) plays a crucial role in the diagnosis and evaluation of thyroid diseases. The current reference measurement procedure (RMP) has been in place for 20 years and is widely adopted by reference laboratories around the world. To enhance the performance of the RMP, we developed and validated a simplified, SI-traceable candidate RMP specifically targeting serum total T3 (TT3) using isotope dilution-liquid chromatography with tandem mass spectrometry (ID-LC–MS/MS). Specifically, T3 reference material was employed as the standard. Compared to the RMP, our method incorporates a simplified serum cleanup process involving protein precipitation and nitrogen drying. The method validation followed ISO guidelines for measurement uncertainty assessment. Our results indicated that there was no significant conversion of T4 into metabolites during the serum pretreatment. The lower limit of the measuring interval was determined to be 0.077 nmol/L, and the regression model was linear across a range of 0.016 to 13.086 nmol/L. The imprecision of intra-assays ranged from 0.1 to 1.9%, while inter-assay imprecision ranged from 0.5 to 1.2%. The bias observed when analyzing SRM971 was between − 0.34 and − 1.65%. This candidate RMP demonstrated excellent agreement with the RMPs developed by RELA activity, showing a mean bias falling within the educational mean ratio (6%). The measurement uncertainties were 0.022 nmol/L for RELA2023A and 0.120 nmol/L for RELA2023B. In conclusion, the developed candidate RMP is traceable, reliable, and easy to operate, showing promising potential for the development of serum reference materials and the standardization of routine assays. Graphical

CAS / MDL: 64365-11-3 18835-59-1
研究领域: 临床检验学 · 内分泌学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF SEPARATION SCIENCE · 2019 ·Vol. 42 ·期 16 ·2592-2601 · IF 2.516

Simultaneous determination of five isoflavones in rat plasma by LC-MS/MS: Comparative pharmacokinetic characteristics of Puerariae lobatae radix in normal and type 2 diabetic rats

Hongmin Zhang,Xintong Hu,Miao Qiao,Yang Li,Shijie Cao,Liqin Ding,Xinchi Feng,Ning Kang,Deqin Zhang,Feng Qiu

A rapid and sensitive liquid chromatography with tandem mass spectrometry method was developed and validated for simultaneous determination of puerarin, daidzin, daidzein, 3′-hydroxy puerarin, and genistein in rat plasma after oral administration of Puerariae lobatae radix extract. The method of protein precipitation with acetonitrile was used for sample preparation. Chromatographic separation was achieved on a C 18 column with the mobile phases of acetonitrile/water containing 0.1% formic acid. The analytes were detected by mass spectrometer with an electrospray ionization source operating in the negative ion mode. The linearity, precision, accuracy, dilution reliability, recovery, matrix effects, and stability of the method were within acceptable ranges. The developed method was successfully used to compare the pharmacokinetic characteristics of five analytes in normal and type 2 diabetics rats after oral administration of Puerariae lobatae radix extract. Several pharmacokinetic alterations were observed and this might be caused by the pathological state of type 2 diabetes.

研究领域: 药理学 · 分析化学 · 糖尿病研究
✓ 已验证 DOI PubMed 高影响因子
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