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蚕沙不同炮制品中黄酮和氨基酸等主要成分的LC-MS/MS分析 被引量:1

LC-MS/MS Analysis of Flavonoids and Amino Acids in Different Fried Silkworm Excrement Products
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摘要 目的比较蚕沙不同炒制品中黄酮类和氨基酸类成分含量。方法采用高效液相色谱串联三重四级杆质谱法(HPLC-MS/MS法)对生蚕沙、炒黄蚕沙、炒焦蚕沙、炒炭蚕沙中2种黄酮类(紫云英苷、异槲皮苷)、1种有机酸(奎宁酸)、1种香豆素类(伞形花内酯)和6种氨基酸(丙氨酸、色氨酸、缬氨酸、亮氨酸、异亮氨酸、苯丙氨酸)进行含量测定,选择色谱柱CAPCELL PAK C18 MGIII(2.0mm×150mm,3μm),流动相10mmol/L甲酸铵+0.1%甲酸水(A)-乙腈溶液(B),梯度洗脱(0~2min,5%B;2~2.5 min,5%~20%B;2.5~6 min,20%~50%B;6~6.1min,50%~80%B;6.1~8 min,80%B;8~8.1 min,80%~5%B;8.1~11 min,5%B),流速为0.3 mL/min,质谱检测方式为多反应监测。结果各类成分在一定范围内具有良好的线性关系,精密度的范围为0.69%~3.12%。另外,蚕沙经炒制后,黄酮类成分与氨基酸类成分含量均发生变化,在炒黄中,紫云英苷、异槲皮苷、丙氨酸、亮氨酸与苯丙氨酸含量下降,色氨酸、缬氨酸与异亮氨酸含量增加;在炒焦蚕沙中,除紫云英苷、异槲皮苷含量有所增加,其他成分均下降;在炒炭蚕沙中,各成分含量均呈现明显下降,其中色氨酸和苯丙氨酸未检出。结论该方法简便、灵敏、检测时间短、精密度高,可用于蚕沙及其炮制品中黄酮类与氨基酸类成分的测定,为进一步研究蚕沙炮制前后化学成分变化奠定基础。 Objective To compare the content of flavonoids and amino acids in different fried silkworm excrement products.Methods HPLC-MS/MS was used to compare 3 kinds of flavonoids(astragalin,isoquercitrin,quinic acid)and 6 kinds of amino acids in raw silkworm excrement,fried yellow silkworm excrement,fried coke silkworm excrement,and charcoal silkworm excrement.Assay components(alanine,tryptophan,valine,leucine,isoleucine,phenylalanine),select the column CAPCELL PAK C18 MGIII(2.0 mm×150 mm,3μm),flow Phase 10 mmol/L ammonium formate+0.1%formic acid water(A)-acetonitrile solution(B),gradient elution(0~2 min,5%B;2~2.5 min,5%~20%B;2.5~6 min,20%~50%B;6~6.1 min,50%~80%B;6.1~8 min,80%B;8~8.1 min,80%~5%B;8.1~11 min,5%B).The flow rate is 0.3 mL/min,spray ion source(Turbo-V),collect data in positive and negative ion modes.Results The above-mentioned 3 kinds of flavonoids and 6 kinds of amino acids had a good linear relationship within a certain range,and the range of precision was 0.69%-3.12%.In addition,after the silkworm excrement is fried,the content of flavonoids and amino acids changes.In the fried process,the content of astragaloside,isoquercitrin,alanine,leucine and phenylalanine decreases.Quinic acid,tryptophan,valine and isoleucine content increased;in the fried coke silkworm excrement,in addition to the content of venetin and isoquercitrin increased,the other components were all decreased;In the silkworm excrement,the content of each component showed a significant decrease.Conclusion The method is simple,sensitive,short in detection time,and high in precision.It can be used for the determination of flavonoids and amino acids in silkworm excrement and its processed products,and lays a foundation for further research on the chemical composition changes of silkworm excrement before and after processing.
作者 熊之琦 付辉政 曹娟 高慧 杨茜 叶喜德 惠艳春 XIONG Zhi-qi;FU Hui-zheng;CAO Juan;GAO Hui;YANG Qian;YE Xi-de;HUI Yan-chun(Affiliated Hospital of Jiangxi University of Chinese Medicine,Nanchang 330004,China;Jiangxi Institute for Drug Control,NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine,Jiangxi Province Engineering Research Center of Drug and Medical Device Quality,Nanchang 330029,China;Jiangxi Provincial Children's Hospital,Nanchang 330006,China;Sanyo Fine Trading Co.,Ltd.Beijing 100176,China)
出处 《时珍国医国药》 CAS CSCD 北大核心 2021年第6期1379-1382,共4页 Lishizhen Medicine and Materia Medica Research
基金 江西省中医药管理局科技计划项目(2019A237) 江西省中医药中青年骨干人才(第一批)培养计划【赣中医药科教字[2020]2号】 江西省学位与研究生教育教学改革研究项目(JXYJG-2019-122)。
关键词 蚕沙 黄酮类成分 氨基酸类成分 LC-MS/MS Silkworm excrement Flavonoids Amino acids LC-MS/MS
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