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作 者:陈云 郁红礼[1,2,3] 吴皓[1,2,3] 王卫[1] 李瑶 程梓烨 单雪莲[1] CHEN Yun;YU Hong-li;WU Hao;WANG Wei;LI Yao;CHENG Zi-ye;SHAN Xue-lian(School of Pharmacy,Nanfing University of Chinese Medicine,Nanjing 210023,China;Jiangsu Key Laboratory of Chinese Medicine Processing,Nanjing 210023,China;Engineering Center of State Ministry of Education for Standardization of Chinese Medicine Processing,Nanjing 210023,China)
机构地区:[1]南京中医药大学药学院,江苏南京210023 [2]江苏省中药炮制重点实验室,江苏南京210023 [3]国家教育部中药炮制规范化及标准化工程研究中心,江苏南京210023
出 处:《中国中药杂志》2018年第22期4457-4461,共5页China Journal of Chinese Materia Medica
基 金:《中国药典》2020年版标准提高项目
摘 要:考察以猪胆汁为原料的胆南星发酵炮制品及混合蒸制炮制品中主要胆汁酸类成分的组成,建立发酵制胆南星中胆汁酸类成分的含量测定方法。以猪胆汁及天南星、制天南星为原料分别制备发酵法胆南星及混合蒸制法胆南星,采用HPLC-ELSD检测比较2种胆南星中胆汁酸类成分的差异;以3种游离胆汁酸类成分为指标,采用HPLC-ELSD检测发酵制胆南星炮制品中的胆汁酸类成分的含量。采用Agilent Eclipse XDB C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-0.1%冰醋酸水(55∶45)为流动相,流速为1 mL·min^-1,柱温为30℃,ELSD:漂移管温度为90℃,氮气流量为2.2 mL·min^-1。结果显示混合蒸制法胆南星中主要含有结合型胆汁酸类成分,发酵制胆南星中未见有结合型胆汁酸类成分,主要含游离型胆汁酸类成分。发酵制品中的3种游离型胆汁酸类成分猪胆酸(HCA)、猪去氧胆酸(HDCA)和鹅去氧胆酸(CDCA)均在定量范围内呈良好的线性关系,平均加样回收率在95.99%104.3%,加样回收符合要求。研究结果表明,胆南星发酵过程可使得胆汁中的结合型胆汁酸类成分转化为游离型胆汁酸。所建方法可以有效控制发酵制胆南星中胆汁酸类成分的含量。The aim of this study is to analyze the compositions of main bile acids in fermented and mixed processing products of arisame cum bile from pig bile,and to establish a method for content determination of bile acids in fermented Arisaema Cum Bile.Fermented and mixed processing products were prepared from arisaematis rhizome and arisaematis rhizoma preparatum with pig bile respectively.Then the differences in bile acids compositions between such two kinds of products were compared by high performance liquid chromatography and evaporative light-scattering detector(HPLC-ELSD).With three kinds of free bile acid compositions as the indicators,HPLC-ELSD method was adopted to determine the content of bile acid compositions in fermented product,on Agilent Eclipse XDB C18(4.6 mm×250 mm,5μm)chromatographic column,with acetonitrile and 0.1%glacial acetic acid solution(55∶45)as mobile phase,at a flow rate of 1 mL·min-1,column temperature of 30℃,drift tube temperature of 90℃,and a nitrogen flow rate of 2.2 mL·min-1.The results showed that the bile acids in fermented bile Arisaema were mainly in a free form,while in mixed processing product,the compositions were mainly in a conjugated form.Three kinds of free bile acids,namely porcine cholic acid(HCA),porcine deoxycholic acid(HDCA)and chenodeoxycholic acid(CDCA)in fermented product,showed a good linear relationship in the range of quantification.The average recovery rate was 95.99%-104.3%,complying with the requirements.The results showed that the conjugated bile acids could be transformed into free bile acids during the fermentation of arisaema cum bile.This established method can effectively control the content of bile acids compositions in fermenting arisaema cum bile.
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