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FOOD AND AGRICULTURAL IMMUNOLOGY · 2021 · IF 3.101

A magnetic-separation-based homogeneous immunosensor for the detection of deoxynivalenol coupled with a nano-affinity cleaning up for LC-MS/MS confirmation

Jie-Biao Guo,Tai-Long Wei,Qing-Hua He,Jin-Sheng Cheng,Xiu-Zhen Qiu,Wang-Pei Liu,Xian-Quan Lan,Lu-Fen Chen,Min Guo

A magnetic separation-based immunosensor for deoxynivalenol assay, coupled with a nano-affinity cleaning up for instrumental confirmation, was developed. Maltose-binding protein with mimic epitope of DON was coupled to CdSe/ZnS quantum dot nanobeads for fluorescent reporter. Graphene oxide was linked with magnetic nanoparticles and protein G for immunomagnetic adsorbent. The magnetic separation of reporter could be inhibited by DON so the fluorescent remained in the solution indicates a good quantitative correlation to DON concentration. The DON separated by immune adsorbent can be cleaned up for instrumental confirmation. The optimized immunosensor showed results as follows: the linear range was in 0.3–3000 ng mL−1. The limits of detection (S/N = 3) were 0.50, 1.0, and 3.0 ng mL−1 in different backgrounds. The recoveries for DON-spiked samples range from 78.7% to 88.5%. Both results of UPLC-MS/MS based on affinity column purification and coupled with nano-affinity cleaning up showed a good agreement with the current immunosensor.

研究领域: 食品安全检测 · 免疫学 · 分析化学
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2023 · IF 3.4

Development and validation of a sensitive and simple LC-MS/MS method for simultaneous quantitation of valsartan, sacubitril and sacubitrilat in pediatric population

Quancheng Yang,Peng Cao,Yi Lv,Hua Peng,Xuejia Zhai

Pediatric heart failure (HF) is an important clinical disease with high hospitalization rates, morbidity, mortality and medical costs. Sacubitril/valsartan (also known as Entresto), was approved for the treatment of adult HF and is recently used in pediatrics. However, clinical therapy on children is more challenging than adults, and the pharmacokinetics of Entresto in children are still largely unknown and urgently needed. Herein, we aim to develop a simple and sensitive analytic method to monitor Entresto in pediatric patients, which is of great importance for individualized safe medication in children. Specifically, a liquid chromatography tandem mass spectrometry method for simultaneously quantification of valsartan, sacubitril and its bio-active metabolite sacubitrilat in human plasma has been developed and validated in pediatric patients. Plasma samples were pretreated with acetonitrile for protein precipitation. Elution was performed on X Select HSS T3 column (2.1 × 100 mm, 5 µm; Waters) column using an isocratic mobile phase process consisting of 0.1% formic acid aqueous solution and 0.1% formic acid acetonit rile with a total run time of 3.0 min. Valsartan-d3, sacubitrilin-d4 and sacubitrilat-d4 were used as the corresponding deuterium internal standards. According to the Bioanalytical Method Validation Guidance for Industry, the method was validated in the range of 0.5–5000 ng/mL. Intra- and inter-day accuracy of sacubitril,valsartan and sacubitrilat ranged from 93%− 108%, 98%− 109%, 91%− 102%, respectively, with relative standard deviation of precision ranging from 2.0% to 5.1%, 2.4%− 7.5%, 1,3%− 7.4%. The proposed method demonstrated good accuracy, precision and linearity. The matrix factors normalized by internal standard meet the acceptance criteria. The method was fully validated and applied in 39 children. Trough concentration of the three substances to be measured were: valsartan (11.3–938.0 ng/mL), sacubitril (0.5–395.5 ng/mL) and sacubitrilat (522.1–4890.0 ng/mL). Overall, this is the first study to simultaneously determined the plasma valsartan, sacubitril and sacubitrilat concentrations in children, which is believed to facilitate the clinical management of pediatric HF.

CAS / MDL: 64-18-6
研究领域: 药理学 · 儿科学 · 临床医学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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INTERNATIONAL JOURNAL OF FOOD SCIENCE AND TECHNOLOGY · 2024 · IF 2.6

Identification and molecular mechanisms of novel antioxidant peptides in black soldier fly larvae protein: simulated gastrointestinal digestion, molecular docking and in vitro/in vivo studies

Wangxiang Huang,Chen Wang,Qianzi Chen,Feng Chen,Haohan Hu,Jianfei Li,Jingling Kang,Qiyi He,Xiaodong Yu

Summary This study aims to identify novel antioxidant peptides within black soldier fly larvae protein (BSFLP) using simulated gastrointestinal processes, LC–MS/MS analysis, and virtual screening. Two peptides, PFCPK and ADFW, exhibited significant antioxidant properties in both in vitro radical scavenging experiments and in vivo evaluations using zebrafish embryos induced with 2,2′-azobis(2-methylpropionamidine) dihydrochloride. Treatment with 25 μg mL −1 of PFCPK or ADFW significantly ( P < 0.05) enhanced zebrafish embryo survival, reduced abnormal heartbeats and lowered ROS generation rate by 62.98% and 83.44%, lipid peroxidation by 52.54% and 68.35%, and cell death rate by 86.92% and 97.54%, respectively. Moreover, they restored antioxidant enzyme activities and MDA levels to near-normal values, demonstrating significant therapeutic effects. The observed antioxidant effects may potentially be linked to the modulation of the Keap1/Nrf2 pathway. This study provides valuable insights for developing novel natural antioxidants and maximising the high-value applications of BSFLP.

研究领域: 食品科学 · 生物化学 · 分子生物学 · 药理学
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Journal of Functional Foods · 2016 · IF 3.973

Chemical profiles, antioxidant and anti-obesity effects of extract of Bambusa textilis McClure leaves

Meng-Hua Liu,Chun-Hay Ko,Na Ma,Pei-Wen Tan,Wei-Ming Fu,Jing-Yu He

Bambusa textilis McClure ( Bambusoideae ) is a valuable bamboo species widely distributed in southern China. The methanolic extract of B. textilis leaves was examined for its chemical and bioactive properties. As a result, 38 compounds, including organic acids, flavonoids and miscellaneous substances, were identified or tentatively characterised by UFLC-DAD-Q-TOF-MS. Thirteen polyphenols, considered as the most important components, were quantified using LC-MS/MS method. Moreover, the methanolic extract of B.   textilis leaves had obvious antioxidant and anti-obesity activities in vivo in a high-fat diet rat model. It also had a significant antioxidant effect in 2,2-diphenyl-1-picrylhydrazyl (DPPH), ferric reducing antioxidant power (FRAP) and inhibition of β-carotene bleaching assays in vitro . These results are useful for further research of B .  textilis leaves that may be useful candidates for the development as a functional food ingredient in health-related industries.

CAS / MDL: 491-70-3 121-34-6
研究领域: 药理学 · 营养学 · 生物化学
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2023 · IF 6

Molecular networking and equivalently quantitative ion strategy for discovery and quantification of glucosinolates in cauliflower and broccoli by liquid chromatography tandem mass spectrometry

E. Hengchao,Shuting Peng,Zhiyong Zhao,Xueqin Yao,Yanmei Zhang,Xiaobei Li,Xianli Yang,Tingting Fan,Xiaoyan Zhao,Changyan Zhou

Glucosinolates (GSLs) are unique secondary metabolites in cauliflower and broccoli, which have diverse biological activities. In this study, a molecular networking combined with the equivalently quantitative ion strategy was built based on liquid chromatography tandem mass spectrometry (LC-MS/MS) for the discovery and quantification of GSLs in cauliflower and broccoli. Firstly, 19 GSLs were identified including 2 new compounds, 4-hydroxyneoglucobrassicin and gluco-4-hydroxyneoglucobrassicin. Moreover, the shared fragment ion m/z 96.0 was set as the equivalently quantitative ion to quantify GSLs. This method could use only one reference standard (or one calibration curve) to efficiently quantify all aliphatic and phenyl GSLs in cauliflower and broccoli. This method was fully validated with good linearity, recovery and sensitivity, and subsequently applied in GSLs quantification. The developed strategy could also be applied in GSLs discovery and quantification in other Brassicaceae vegetables.

CAS / MDL: 631-61-8
研究领域: 分析化学 · 食品科学 · 植物科学 · 植物化学
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JOURNAL OF ETHNOPHARMACOLOGY · 2024 · IF 4.8

Determination of arbutin in vitro and in vivo by LC-MS/MS: Pre-clinical evaluation of natural product arbutin for its early medicinal properties

Qiao-Lai Wang,Pei-Xi Zhang,Rui Shen,Meng Xu,Liang Han,Xuan Shi,Zi-Rui Zhou,Jing-Yi Yang,Jie-Qing Liu

Ethnopharmacological relevance Arbutin is a naturally occurring glucoside extracted from plants, known for its antioxidant and tyrosinase inhibiting properties. It is widely used in cosmetic and pharmaceutical industries. With in-depth study of arbutin, its application in disease treatment is expanding, presenting promising development prospects. However, reports on the metabolic stability, plasma protein binding rate, and pharmacokinetic properties of arbutin are scarce. Aim of the study The aim of this study is to enrich the data of metabolic stability and pharmacokinetics of arbutin through the early pre-clinical evaluation, thereby providing some experimental basis for advancing arbutin into clinical research. Materials and methods We developed an efficient and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay for determining arbutin in plasma. We investigated the metabolic and pharmacokinetic properties of arbutin through in vitro metabolism assay, cytochrome enzymes P450 (CYP450) inhibition studies, plasma protein binding rate analysis, Caco-2 cell permeability tests, and rat pharmacokinetics to understand its in vivo performance. Results In vitro studies show that arbutin is stable, albeit with some species differences. It exhibits low plasma protein binding (35.35 ± 11.03% ∼ 40.25 ± 2.47%), low lipophilicity, low permeability, short half-life (0.42 ± 0.30 h) and high oral bioavailability (65 ± 11.6%). Arbutin is primarily found in the liver and kidneys and is eliminated in the urine. It does not significantly inhibit CYP450 up to 10 μM, suggesting a low potential for drug interactions. Futhermore, preliminary toxicological experiments indicate arbutin's safety, supporting its potential as a therapeutic agent. Conclusion This study provides a comprehensive analysis the drug metabolism and pharmacokinetics (DMPK) of arbutin, enriching our understanding of its metabolism stability and pharmacokinetics properties, It establishes a foundation for further structural optimization, pharmacological studies, and the clinical development of arbutin.

研究领域: 药理学 · 分析化学 · 临床前研究
✓ 已验证 产品关联 DOI PubMed 高影响因子
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PeerJ · 2021 · IF 2.984

Simultaneous determination of two galangin metabolites from Alpinia Officinarum Hance in rat plasma by UF LC-MS/MS and its application in pharmacokinetics study

Rangru Liu,Hailong Li,Na Wei,Yinfeng Tan

Galangin has multiple pharmacological efficacies, such as anti-cancer, anti-inflammation and anti-oxidation. Galangin can be rapidly converted into glucuronidated metabolites in vivo. This study aimed to establish an UFLC-MS/MS analytical method to simultaneously determine the concentrations of two glucuronidated metabolites of galangin, galangin-3-O-β-D-glucuronic acid (GG-1) and galangin-7-O-β-D-glucuronic acid (GG-2) in rat plasma. After oral administration of galangal extract (0.3 g/kg), blood samples were collected from the orbital sinus, then treated by methanol precipitation and further gradient-eluted with Phenomenex Kinetex 2.6 µm XB-C18 column. The mass spectrometer was manipulated in the negative electrospray ionization (ESI) and selected multiple reaction monitoring (MRM) mode for the analytes. The precursor-to-product ion pairs applied for GG-1, GG-2 and chrysin (as the internal standard, IS) were m/z 445.2→269.0, 445.2→268.9 and 253.0→142.9, respectively. The results showed that the linear ranges for both GG-1 and GG-2 were 2.0–2000.0 ng/mL ( r 2 > 0.995). The inter- and intra-day precision were 89.3%–109.2%, RSD was less than 15%, and the repeatability was good. The recoveries of both metabolites and IS were over 89%, and matrix effect was within 15%. The validated analytical method was further applied to study the pharmacokinetic profiles of GG-1 and GG-2 in vivo. The pharmacokinetic parameters suggested that T max of GG-1 was equivalent to that of GG-2, and MRT 0-t , t 1/2 of GG-2 were a little higher than those of GG-1. Importantly, AUC 0-t and C max of GG-2 were almost twice as those of GG-1. In short, the validated UFLCMS/MS analytical method was feasible to simultaneously determine two galangin metabolites GG-1 and GG-2 in rat plasma and further analyze in vivo metabolism of galangin.

研究领域: 药物分析 · 药理学 · 生物化学
✓ 已验证 DOI 高影响因子
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Metabolites · 2026 ·Vol. 16 ·期 8 ·543 · IF 4.5

Spatial Metabolomics Reveals Microregion-Specific Neurochemical Perturbations in the Brains of PCPA-Induced Insomniac Rats: Integration of MALDI-MSI and Targeted LC-MS/MS

Yan Yan,Jiaying Liu,Yingjian Deng,Yu Tao,Xinxin Li,Chenhui Du,Kun Yang,Ruiping Zhang

Objectives:Insomnia is a highly prevalent sleep disorder involving complex neurochem-ical dysregulation; however, the spatial distribution of neurotransmitters and small-molecule metabolites across distinct brain microregions in the insomniac state re-mains poorly characterized. This study aimed to map region-specific metabolic perturba-tions in situ in a p-chlorophenylalanine (PCPA)-induced insomnia rat model using opti-mized matrix-assisted laser desorption/ionization mass spectrometry imaging (MAL-DI-MSI) integrated with targeted metabolomics validation.Methods:On-tissue chemical derivatization MALDI-MSI was optimized using α-cyano-4-hydroxycinnamic acid (CHCA) as the matrix on a Bruker tims TOF flex mass spectrometer. The rats received PCPA (400 mg/kg, intraperitoneal) for three days to establish the insomnia model. Metabolite identifi-cation was conducted using MetaboScape® software (2020b) and the Human Metabolome Database. Ultra-performance liquid chromatography–tandem mass spectrometry was em-ployed to quantify nine key neurotransmitters and metabolites across six brain microre-gions. Key synthetic enzyme expression was evaluated by immunofluorescence and West-ern blotting analyses.Results:TMP-TFB-derived brain slices clearly showed the distribu-tion of neurotransmitters in brain microregions. MALDI-MSI demonstrated that the spatial distribution and abundance of eight neurotransmitters were disturbed in brains of PCPA-induced insomniac rats. A total of 346 metabolites were characterized across six brain microregions (cerebellum, cortex, hippocampus, brainstem, hypothalamus, and stri-atum), with principal coordinate analysis revealing clear metabolic separation between control and insomniac rats. PCPA treatment markedly disrupted tryptophan and tyrosine metabolism, evidenced by decreased 5-HT, 5-HTP, and 5-HIAA, alongside region-specific alterations in DA, NE, HVA, and Ach. Additionally, GABA levels decreased in the hippo-campus, striatum, and hypothalamus, whereas glutamate increased throughout the brain. Targeted metabolomics validated the MSI findings, and Bland–Altman analysis confirmed good consistency between the two analytical platforms. PCPA further disturbed the meta-bolic enzymes MAOA, DDC, and TPH2 within the Trp-5-HTP-5-HT-5-HIAA metabolic pathway in the brainstem and TYH and DBA within the tyrosine-DA-NE metabolic pathway in the striatum.Conclusions:This study demonstrates that region-specific altera-tions in tryptophan and tyrosine metabolism pathways provide mechanistic insights into insomnia pathogenesis and potential therapeutic targets.

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BMC Chemistry · 2026 · IF 5.1

Development of a novel LC-MS/MS method for concurrent determination of imipenem, relebactam, and cilastatin in human serum, urine and peritoneal drainage fluid

Yang Xiaoyu,Zhao Chaoyue,Ding Yiwen,Li Yining,Zhao Yushang,Lin Wanling,Li Jing,Wang Dong,Yue Zhihong,Pei Lin,Jia Mei,Cao Lin-Lin,Wang Hui

With the global spread of antimicrobial resistance (AMR), infections caused by multidrug-resistant bacteria have become a major challenge in clinical treatment. ‘Imipenem, Cilastatin Sodium and Relebactam for Injection’ is a critical therapeutic agent for treating infections caused by multidrug-resistant Gram-negative bacteria. However, it is associated with gastrointestinal adverse reactions, necessitating therapeutic drug monitoring (TDM) for precise dosing. Currently, there is no method for simultaneously detecting the concentrations of all three components in ‘Imipenem, Cilastatin Sodium and Relebactam for Injection’. Therefore, this study established an analytical method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous quantification of imipenem, relebactam, and cilastatin in serum, urine, and peritoneal drainage fluid (PD). After protein precipitation, samples were separated using a CORTECS ® HILIC column with 5 mM ammonium acetate aqueous solution-acetonitrile as the mobile phase for gradient elution, detected in positive electrospray ionization (ESI+) mode. This LC-MS/MS method showed excellent linearity (R² > 0.99) for all three drugs, and the linearity ranges had well met the clinical requirements. The limits of quantification (LOQ) were 40 ng/mL (serum/ PD) and 80 ng/mL (urine), and the carryover contamination rate was < 0.1%. All intra-day and inter-day coefficients of variation (CVs) were < 15%, the recovery rates ranged from 89.7% to 103.2%, and the matrix effects were acceptable (87.7%–110.8%). In conclusion, this LC-MS/MS method is simple to operate, exhibits high sensitivity and accuracy, and meets the requirements for the TDM of ‘Imipenem, Cilastatin Sodium and Relebactam for Injection’, providing support for individualized treatment and reducing the risk of adverse reactions.

✓ 已验证 DOI PubMed 高影响因子
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Analytical Methods · 2026 · IF 3

Development and validation of an LC-MS/MS/MS method for the sensitive quantification of trace β-agonists in complex animal-derived food matrices

Chujun Liu,Jiankang Ren,Qian Ran,Yuliang Xu,Boyan Sun,Zhiyue Feng,Sihan Wang,Jie Xie,Haiyang Jiang

Conventional multiple reaction monitoring (MRM) quantification of β-agonists in complex matrices was hindered by insufficient sensitivity due to co-extracted matrix interferences. To address this drawback, we developed a highly selective and specific liquid chromatography triple-stage tandem mass spectrometry (LC-MS/MS/MS, LC-MS3) method via systematic comparison of MRM and MRM3 modes for the determination of nine β-agonists (ractopamine, penbutolol, cimaterol, salbutamol, clenbuterol, tulobuterol, clorprenaline, terbutaline, fenoterol) in high-fat milk and pork. MS3 method overcomes the limitations of conventional MS/MS through the multi-stage fragmentation capability of a hybrid linear ion trap (LIT), enabling deeper structural characterization and superior matrix interference resistance. The results demonstrated that LC-MS3 method not only accurately quantified β-agonists in complex matrices, but also significantly enhanced sensitivity by reducing matrix effects. Extracted ion chromatograms (XICs) revealed nearly interference-free peaks, exhibiting the excellent selectivity and specificity of the LC-MS3 method. The LC-MS3 method exhibited good linearity (R² ≥ 0.9973), and the limits of detection (LOD) and quantification (LOQ) for β-agonists ranged from 0.01 to 0.05 μg/kg and 0.03 to 0.15 μg/kg, respectively. The recoveries were between 85.47% and 105.32%, with intra-day and inter-day relative standard deviations (RSDs) of 1.68%–6.42% and 2.42%–8.68%, respectively. The matrix effect (ME) was within -10.55% to 9.53%. In comparison, the conventional LC-MS/MS method showed higher LODs (0.1–0.15 μg/kg), LOQs (0.3–0.45 μg/kg), and broader matrix effects (-18.12%–19.35%), confirming the superior sensitivity of the LC-MS3 method. This is the first study to employ MRM3 mode for the determination of β-agonists in high-fat milk and pork matrices.

✓ 已验证 DOI PubMed 高影响因子
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CHIRALITY · 2026 ·Vol. 38 ·期 3 ·e70091 · IF 2.4

Simultaneous Separation and Determination of Chiral Amino Acids and Histamine in Doenjang by LC–MS/MS Based on a Novel Chiral Derivatization Probe Labeling

Mengwei Zhang,Shuyi Song,Yingao Wang,Songze Wang,Mingshan Zheng,Xi-Ling Li,Jun Zhe Min

Doenjang is the most used fermented soy product in Asian countries. At present, the simultaneous determination of DL-amino acids and histamine in doenjang has not been reported. Therefore, an UHPLC–MS/MS method was developed based on a novel chiral derivatization probe DBD-M-Pro, enabling for the first time the simultaneous quantification of 10 DL-amino acids and histamine in doenjang samples from different regions. Achieving resolution (Rs) values of 1.62–6.31 for the 10 DL-amino acids. The limits of detection (LODs) for DL-amino acids and histamine ranged from 0.54 to 15.62 pmol. The intraday and interday precision (RSD) were 0.21%–10.63%, and the average recoveries were 93.18%–109.07%. This method was applied to analyze 12 doenjang samples from Northeastern China, Korea, and Japan. The results showed that there was a significant geographical distribution of DL-amino acids and histamine. Yanbian Korean doenjang from China showed a unique advantage in that the total amount of DL-amino acids was significantly higher than that from other regions, with histamine concentration generally increasing with longer fermentation times. This study provides a stable and reliable method for the simultaneous determination of chiral amino acids and histamine in fermented foods such as doenjang.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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Frontiers in Nutrition · 2025 · IF 5.1

Development of an LC-MS/MS method for astaxanthin quantification in shrimp tissues and its application to detect astaxanthin variations during ovary development stages

Shuo Diao,Guanrong Feng,Yixuan Wang,Jingming Ma,Zhihua Lv,Mingming Yu,Yue Sun

Objective: In this study, a highly selective and sensitive LC-MS/MS method was developed to comprehensively analyze the distribution of astaxanthin across various tissues of Litopenaeus vannamei, as well as its variations in the hepatopancreas and ovary throughout ovarian development.Methods: The separation was performed on a BEH C8 column (1.7 μm, 2.1 × 50 mm) using a a gradient elution. The initial mobile phase composition was 0.1% formic acid in 3 mM ammonium acetate in water (solvent A) and methanol (solvent B) at a ratio of 15:85 (v/v), with a flow rate of 0.20 mL/min.Results: The assay demonstrated linearity over a concentration range of 20 to 10,000 ng/mL, with accuracy varying from −0.1 to 1.7% and precision within 2.1%. Using the established methodology, astaxanthin concentrations were quantitatively analyzed and comparatively assessed across various tissues of L. vannamei. Analytical results demonstrated that the ventral nerve cord and hepatopancreas exhibited the highest astaxanthin concentrations among all examined tissues, with values of 351 μg/g and 116 μg/g, respectively. During the ovarian developmental stages, astaxanthin was predominantly sequestered in the hepatopancreas during early phases, with concentrations ranging from 21.3 μg/g to 29.1 μg/g, representing a 43- to 59-fold increase compared to ovarian concentrations. However, a significant redistribution of astaxanthin was observed during the post-developmental stage, characterized by a substantial decrease to 5.74 μg/g in the hepatopancreas, concomitant with an increase to 7.47 μg/g in ovarian tissue.Conclusion: This validated LC-MS/MS method effectively quantified astaxanthin in various tissues of Litopenaeus vannamei, providing new insights into its tissue-specific distribution and potential role during ovarian development.

CAS / MDL: 472-61-7 631-61-8
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