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Food Bioscience · 2024 · IF 4.8

Determination of bisphenols in food and its contact materials migration by magnetic solid-phase extraction coupled with LC-MS/MS

Cheng Yang,Yan Wang,Pei-Zhi Dong,Yanan Li,Yue-Hong Pang

Bisphenols (BPs) pose a pervasive threat to human health due to their potential to leach from plastic packaging into food, thereby endangering the endocrine system. Given their low concentrations in complex samples, the development of a swift, efficient pretreatment method is imperative. In this study, a magnetic covalent organic framework (Fe 3 O 4 @TzDa) was synthesized via a layer-by-layer growth approach, utilized in rapid magnetic solid-phase extraction (MSPE) combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination BPs. This method exhibited remarkable sensitivity, detecting five BPs (BPS, BPF, BPA, BPB, and BPAF) at levels between 0.68 and 0.77 μg L −1 . Fe 3 O 4 @TzDa nanocomposites maintained an extraction efficiency of approximately 98.0% over five cycles, ensuring robust and repeatable performance. Sample analysis, encompassing plastic bottled water, pear juice, mix juices, pop-top canned curry beef, and box-packed milk, yielded recoveries of 72.0%–114.0% (RSDs <7.5%, n  = 5). Furthermore, BPs migration in sports cups and portable bottles was evaluated, revealing migration levels ranging from 0.0014 to 0.0058 mg kg −1 . This study advances BP analysis by introducing a reliable method for their efficient determination in beverage samples from plastic food packages. The utilization of Fe 3 O 4 @TzDa underscores a pivotal advancement in sample preparation, enhancing both sensitivity and efficiency for the extraction and determination of BPs in food samples.

研究领域: 食品安全 · 分析化学 · 环境科学
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2024 · IF 3.1

Targeted LC-MS/MS method of oxylipin profiling reveals differentially expressed serum metabolites in type 2 diabetes mice with panaxynol

Xina Yu,Shanshan Song,Zhanhua Li,Tiantian Wang,Hui Huang,Qing Shen,Zongyuan Wu,Pei Luo

Panaxynol is a bioactive polyacetylene in food plants; however, its specific benefits in diabetes and metabolic disorders remain unclear. Previous studies have mainly focused on biochemical indicators and clinical evaluations. Limited research has systematically elucidated the beneficial effects of panaxynol from the oxylipins perspective. In this study, we employed an oxylipin analysis platform we previously established using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) based on the multiple reaction monitoring (MRM) method for the profiling of oxylipins. After a 7-week administration of panaxynol to db/db mice, significant alterations in serum oxylipins and potential benefits to hyperglycemia, insulin resistance, and hepatic steatosis were observed. Our analysis also revealed correlations among epoxygenase products derived from arachidonic acid (AA), linoleic acid (LA), and α-linolenic acid (ALA) via cytochrome P450 (CYP) pathways. Furthermore, six potential oxylipins were identified, as offering insights into the mechanisms by which panaxynol may modulate diabetes. These results provide the first in vivo evidence of the impact of panaxynol on oxylipin metabolism and lay the foundation for developing panaxynol as a nutraceutical for diabetes management.

CAS / MDL: 1634-04-4
研究领域: 代谢组学 · 营养学 · 药理学
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JOURNAL OF PHOTOCHEMISTRY AND PHOTOBIOLOGY B-BIOLOGY · 2024 · IF 3.9

LC-MS/MS-based targeted carotenoid and anthocyanidin metabolic profile of Auricularia cornea under blue and red LED light exposure

Lei Ye,Xin Li,Lingzi Zhang,Yu Huang,Bo Zhang,Xuezhen Yang,Wei Tan,Xiaolin Li,Xiaoping Zhang

Light exposure significantly impacted the coloration and metabolism of Auricularia cornea , although the underlying mechanisms remain unclear. This study aimed to test the apparent color and pigment metabolic profiles of A. cornea in response to red (λp = 630 nm) and blue (λp = 463 nm) visible light exposure. Colorimeter analysis showed that fruiting bodies appeared bright-white under red-light and deeper-red under blue-light, both with a yellow tinge. On the 40th day of light-exposure, bodies were collected for metabolite detection. A total of 481 metabolites were targeted analysis, resulting in 18 carotenoids and 11 anthocyanins. Under red and blue light exposure, the total carotenoids levels were 1.1652 μg/g and 1.1576 μg/g, the total anthocyanins levels were 0.0799 μg/g and 0.1286 μg/g, respectively. Four differential metabolites and three putative gene linked to the visual coloration of A. cornea were identified. This pioneering study provides new insights into the role of light in regulating A. cornea pigmentation and metabolic profile.

CAS / MDL: 128-37-0
研究领域: 真菌学 · 代谢组学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2026 · IF 2.5

Enhancing detection efficiency of RD-proteins in Mycobacterium tuberculosis culture filtrate by biomimetic affinity chromatography coupled with LC-MS/MS

Yingxiao Han,Songwei Ma,Rui Ma,Jingjing Li,Lei Qiu,Jia wen Ma,Yanyan Ma,Mengyin Tang,Zhijuan Cao,Ziqi Li,Shulin zhang,Guorong Ma

Mycobacterium tuberculosis culture filtrate proteins (MTB-CFPs) are critical for tuberculosis diagnosis and vaccine development. To explore their diagnostic potential, MTB was statically cultured in Sauton's medium for 15 days; MTB-CFPs were collected, fractionated using six biomimetic affinity chromatography (BiAC) resins, and analyzed by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS). Four MTB-specific regions of difference (RDs) and the PstS1 protein were recombinantly expressed and purified, with their serological efficacy assessed by ELISA using sera from 157 pulmonary tuberculosis (pTB) patients and 71 healthy controls (HCs). LC-MS/MS identified 622 MTB proteins, 307 of which were validated with ≥2 peptides and P  < 0.05. BiAC fractionation significantly increased the average peptide number (2.09-fold), peptide coverage (1.43-fold), and the exponentially modified Protein Abundance Index (emPAI) (1.70-fold) in 281 common identifications. Receiver Operating Characteristic (ROC) analysis revealed rEC (a fusion expression product of the Rv3875 and Rv3874 genes in the RD1 region, linked by a 15-nucleotide connector) as the optimal diagnostic marker Area Under the Curve (AUC = 0.8030), with sharply distinct IgG levels between pTB patients and HCs ( P  < 0.0001). Notably, rEC combined with GmdA (encoded by the Rv1511 gene located in RD11) enhanced sensitivity while preserving high specificity, especially for Acid-Fast Bacilli (AFB) negative pTB cases demonstrating substantial clinical translation potential. Additionally, extended culture promoted MTB autolysis and cytoplasmic protein release, providing valuable insights into TB pathogenesis and biomarker discovery. This integrated approach of BiAC fractionation, proteomics, and serological validation advances TB precision diagnostics.

✓ 已验证 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2019 · IF 2.813

The determination of patulin from food samples using dual-dummy molecularly imprinted solid-phase extraction coupled with LC-MS/MS

Minjuan Zhao,Hua Shao,Yahui He,Hui Li,Mengmeng Yan,Zejun Jiang,Jing Wang,A.M. Abd El-Aty,Ahmet Hacımüftüoğlu,Feiyan Yan,Yanli Wang,Yongxin She

A molecularly imprinted polymer (MIP) with specific adsorption for patulin was successfully polymerized by precipitation polymerization using 2-oxindole (2-oxin) and 6-hydroxynicotinic acid (6-HNA) as dummy template molecules, methylacrylic acid (MAA) as a functional monomer , trimethylolpropane trimethacrylate (TRIM) as a crosslinker, 2,2-azobis-(2-methylpropionitrile) (AIBN) as a initiator, and methanol as a porogen solvent. The molecularly imprinted solid phase extraction (MI-SPE) column was prepared using the polymer as a sorbent and applied for the selective extraction of patulin from real samples. The results showed that the MI-SPE method had high selectivity and specific adsorption towards patulin with mean recoveries ranged between 81.3% and 106.3% and a relative standard deviation (RSD) < 4.5%. Additionally, the developed MI-SPE method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) exhibited good linearity in the range of 1–100 ng mL − 1 with correlation coefficients ( R 2 ) >0.998. The limits of detection (LODs, S/N = 3) were 0.05–0.2 ng g − 1 , and the limits of quantification (LOQs, S/N = 10) were 0.2–0.5 ng g − 1 . The developed method showed a better purification and higher patulin recovery for real samples than the quick, easy, cheap, effective, rugged, safe “QuEChERS” method.

CAS / MDL: 79-41-4 3290-92-4
研究领域: 食品安全检测 · 分析化学
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FOOD CHEMISTRY · 2019 · IF 5.399

Simultaneous determination of tocopherols, carotenoids and phytosterols in edible vegetable oil by ultrasound-assisted saponification, LLE and LC-MS/MS

Liangxiao Zhang,Sujun Wang,Ruinan Yang,Jin Mao,Jun Jiang,Xiupin Wang,Wen Zhang,Qi Zhang,Peiwu Li

A method was developed to simultaneously determine eight bioactive compounds in edible oil based on ultrasound-assisted saponification, liquid-liquid extraction and liquid chromatography coupled with tandem mass spectrometry. Central composite design was employed to optimize ultrasonic temperature and time of saponification. Sample treatment was conducted by ultrasound-assisted saponification at temperature of 75 °C for 40 min. Limits of detection and limits of quantification ranged from 2.0 to 3.2 and from 6.1 to 10.0 ng/mL, respectively. Linear correlations were obtained (R 2  > 0.99) and the recoveries at three spiked levels were between 81.7% and 112.0%. This method was employed to determine eight compounds in camellia oils and olive oils. As results, the contents of stigmasterol, δ-tocopherol, γ-tocopherol, β-carotene and lutein in camellia oils were significantly higher than those in olive oils (p < 0.05). The proposed method can be successfully used to determination of these eight active compounds in camellia oil and other edible oils.

研究领域: 分析化学 · 食品科学 · 生物化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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FORENSIC SCIENCE INTERNATIONAL · 2014 · IF 2.115

Chiral separation and determination of R/S-methamphetamine and its metabolite R/S-amphetamine in urine using LC–MS/MS

Ting Wang,Baohua Shen,Yan Shi,Ping Xiang,Zhiguo Yu

Methamphetamine (MA) and amphetamine (AM) are widely abused drugs. Differentiation of MA and/or AM abuse from therapeutic ingestion of MA and/or AM or one of their precursor drugs is therefore of relevance in clinical and forensic toxicology. The aim of the study was to develop a simple, rapid, and accurate method for the chiral separation and determination of R / S -MA and R / S -AM in urine using liquid chromatography electrospray ionization tandem mass spectrometry operating in the positive ion multiple-reaction monitoring (MRM) mode. 20   μL of urine was diluted 500 times and 20   μL was injected. The chromatographic system consisted of a Chirobiotic™ V2 column (2.1   mm   ×   250   mm, 5   μm), and the mobile phase was methanol containing 0.1% (v/v) glacial acetic acid and 0.02% (v/v) ammonium hydroxide. The method was fully validated through assessments of its linearity (0.05–50.00   mg/L, r 2   >   0.994 for all analytes), and LOQ (0.05   mg/L for all analytes). No matrix effect was observed. The method was successfully applied to 86 urine samples from suspected MA abusers. Only the S -isomers of MA and AM were detected in 72 samples. The concentrations of R -MA ranged from below the LOQ to 13.76   mg/L in 14 urine samples with both enantiomers of MA and/or AM. Pure S -MA is the most common found analyte in urine and principally used by abusers.

CAS / MDL: 1336-21-6
研究领域: 分析化学 · 法医学 · 毒理学
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AAPS Journal · 2013 ·Vol. 16 ·期 1 ·101-113 · IF 4.386

Identification of Key Licorice Constituents Which Interact with Cytochrome P450: Evaluation by LC/MS/MS Cocktail Assay and Metabolic Profiling

Qiao Xue,Ji Shuai,Yu Si-wang,Lin Xiong-hao,Jin Hong-wei,Duan Yao-kai,Zhang Liang-ren,Guo De-an,Ye Min

Licorice has been shown to affect the activities of several cytochrome P450 enzymes. This study aims to identify the key constituents in licorice which may affect these activities. Bioactivity assay was combined with metabolic profiling to identify these compounds in several complex licorice extracts. Firstly, the inhibition potencies of 40 pure licorice compounds were tested using an liquid chromatography/tandem mass spectrometry cocktail method. Significant inhibitors of human P450 isozymes 1A2, 2C9, 2C19, 2D6, and 3A4 were then selected for examination of their structural features by molecular docking to determine their molecular interaction with several P450 isozymes. Based on the present in vitro inhibition findings, along with our previous in vivo metabolic studies and the prevalence of individual compounds in licorice extract, we identified several licorice constituents, viz ., liquiritigenin, isoliquiritigenin, together with seven isoprenylated flavonoids and arylcoumarins, which could be key components responsible for the herb–drug interaction between cytochrome P450 and licorice. In addition, hydrophilic flavonoid glycosides and saponins may be converted into these P450 inhibitors in vivo . These studies represent a comprehensive examination of the potential effects of licorice components on the metabolic activities of P450 enzymes.

CAS / MDL: 62-44-2
研究领域: 药理学 · 分析化学 · 生物化学 · 药学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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WATER RESEARCH · 2022 · IF 13.4

Quantitative identification of halo-methyl-benzoquinones as disinfection byproducts in drinking water using a pseudo-targeted LC-MS/MS method

Jinxiu Lou,Huijie Lu,Wei Wang,Shichong He,Lizhong Zhu

Halobenzoquinones (HBQs) as disinfection byproducts (DBPs) in drinking water is prioritized for research due to their prevalent occurrence and high toxicity. However, only fifteen HBQs can be identified among a high diversity using targeted LC-MS/MS analysis in previous studies due to the lack of chemical standards. In this study, we developed a pseudo-targeted LC-MS/MS method for detecting and quantifying diverse HBQs. Distinct fragment characteristics of HBQs was observed according to the halogen substituent effects, and extended to the development of a multiple-reaction-monitoring (MRM) method for the quantification of the 46 HBQs that were observed in simulated drinking water using non-targeted analysis. The fragmentation mechanism was supported by the changes of Gibbs free energy (ΔG), and a linear relationship between the ΔG and the ionization efficiency of analytes was developed accordingly for quantification of these 46 HBQs, 30 of which were lack of chemical standards. It is noted that 29 of the 30 newly-identified HBQs were halo-methyl-benzoquinones (HMBQs), which were predicted to be carcinogens related with drinking-water bladder cancer risk and be more toxic than non-methyl HBQs. Using the new method, twelve HMBQs were detected in actual drinking water samples with concentrations up to 100.4 ng/L, 3 times higher than that reported previously. The cytotoxicity in CHO cells of HMBQs was over 1-fold higher than that of non-methyl-HBQs. Therefore, HMBQs are an essential, highly toxic group of HBQs in drinking water, which deserve particular monitoring and control.

CAS / MDL: 67-68-5 64-18-6
研究领域: 环境科学 · 分析化学 · 毒理学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2023 · IF 3

Quantification of 10 B vitamins in mouse colon by LC-MS/MS: Application on breast cancer mice treated with doxorubicin

Jing Wu,Yan Xu,Jiahong Yang,Xinyue Yu,Zhaodi Han,Linling Guo,Yin Huang,Yuxin Zhang

B vitamins play important roles in various physiological processes, including cell metabolism and DNA synthesis. The intestine is critical for the absorption and utilization of B vitamins, but few analytical methods for detecting intestinal B vitamins are currently available. In this study, we developed a novel liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous quantification of 10 B vitamins in mouse colon tissue, including thiamin (B1), riboflavin (B2), nicotinic acid (B3), niacinamide (B3-AM), pantothenic acid (B5), pyridoxine (B6), pyridoxal 5′-phosphate (B6-5P), biotin (B7), folic acid (B9), and cyanocobalamin (B12). The method was thoroughly validated following the U.S. Food and Drug Administration (FDA) guidelines and yielded good results in terms of linearity (r 2  > 0.9928), lower limit of quantification (40–600 ng/g), accuracy (88.9–119.80 %) and precision (relative standard deviation ≤ 19.71 %), recovery (87.95–113.79 %), matrix effect (91.26–113.78 %), and stability (85.65–114.05 %). Furthermore, we applied our method to profile B vitamins in the colons of mice with breast cancer after doxorubicin chemotherapy treatment, which revealed that the doxorubicin treatment led to significant colon damage and accumulation of several B vitamins including B1, B2 and B5. We also confirmed the capability of this method for quantifying B vitamins in other intestinal tissues like the ileum, jejunum, and duodenum . The newly developed method is simple, specific, and useful for targeted profiling of B vitamins in mouse colon, with a potential for future studies on the role of these micronutrients in healthy and diseased states.

CAS / MDL: 10294-33-4 10043-11-5
研究领域: 分析化学 · 药理学 · 肿瘤学 · 营养科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2024 · IF 5.7

RNA Adduction Resulting from the Metabolic Activation of Myristicin by P450 Enzymes and Sulfotransferases

Yan He,Zihao Cheng,Jingyu Zhang,Yu Chen,Guode Zhao,Hong Tang,Yufen Liao,Tingmin Ye,Ying Peng,Weiwei Li,Jiang Zheng

Myristicin (MYR) mainly occurs in nutmeg and belongs to alkoxy-substituted allylbenzenes, a class of potentially toxic natural chemicals. RNA interaction with MYR metabolites in vitro and in vivo has been investigated in order to gain a better understanding of MYR toxicities. We detected two guanosine adducts (GA1 and GA2), two adenosine adducts (AA1 and AA2), and two cytosine adducts (CA1 and CA2) by LC-MS/MS analysis of total RNA extracts from cultured primary mouse hepatocytes and liver tissues of mice after exposure to MYR. An order of nucleoside adductions was found to be GAs > AAs > CAs, and the result of density functional theory calculations was in agreement with that detected by the LC-MS/MS-based approach. In vitro and in vivo studies have shown that MYR was oxidized by cytochrome P450 enzymes to 1′-hydroxyl and 3′-hydroxyl metabolites, which were then sulfated by sulfotransferases (SULTs) to form sulfate esters. The resulting sulfates would react with the nucleosides by SN1 and/or SN2 reactions, resulting in RNA adduction. The modification may alter the biochemical properties of RNA and disrupt RNA functions, perhaps partially contributing to the toxicities of MYR.

研究领域: 毒理学 · 药理学 · 分子生物学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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DRUG RESISTANCE UPDATES · 2024 · IF 15.8

Acetate utilization promotes hormone therapy resistance in prostate cancer through neuroendocrine differentiation

Dajun Gao,Yanting Shen,Lingfan Xu,Yi Sun,Hailiang Hu,Bin Xu,Zhong Wang,Huan Xu

Aims Tumor fatty acid (FA) metabolic plasticity plays a pivotal role in resistance to therapy and poses limitations to anticancer strategies. In this study, our aim is to uncover the role of acetate metabolism in neurodifferentiation (NED)-mediated castration-resistant prostate cancer (CRPC). Methods We conducted analyses using LC-MS/MS on clinical prostate cancer tissue before and after hormone therapy. We established tumor xenograft mouse models, primary tumor cells, and human-derived organoids to detect the novel mechanism of NED and to identify potential therapies. Results The hormone therapy-induced upregulation of acetate metabolism was mediated by acyl-CoA synthetase short-chain family member 2 (ACSS2), which increased c-MYC expression for NED induction. Notably, combined treatment with an ACSS2 inhibitor and enzalutamide significantly reduced the xenograft tumor volume. Conclusion Our findings uncovered the critical role of acetate metabolism in NED-mediated CRPC and suggest that ACSS2 inhibitors may represent a novel, low-toxicity strategy when combined with hormone therapy for treating patients with NED-mediated CRPC.

研究领域: 肿瘤学 · 分子生物学 · 癌症代谢 · 前列腺癌 · 激素治疗
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