胶束电动色谱法测定血塞通滴丸5种皂苷类成分及其批次质量一致性评价方法研究  

Determination of five saponins in Xuesaitong Dropping Pills by micellar electrokinetic chromatography and evaluation method of between-batch consistency

作　　者：李淑楠 侯一哲 彭乐 黎翩 蔡翔 李正 李文龙 LI Shu-nan;HOU Yi-zhe;PENG Le;LI Pian;CAI Xiang;LI Zheng;LI Wen-long(College of Pharmaceutical Engineering of Traditional Chinese Medicine,Tianjin University of Traditional Chinese Medicine,Tianjin 301617,China;State Key Laboratory of Component-Based Chinese Medicine,Tianjin University of Traditional Chinese Medicine,Tianjin 301617,China;Langtian Pharmaceutical(Hubei)Co.,Ltd.,Huangshi 435000,China)

机构地区：[1]天津中医药大学中药制药工程学院,天津301617 [2]省部共建组分中药国家重点实验室,天津301617 [3]朗天药业(湖北)有限公司,湖北黄石435000

出　　处：《中国中药杂志》2021年第22期5832-5838,共7页China Journal of Chinese Materia Medica

基　　金：天津市科技计划项目(20ZYJDJC00090)。

摘　　要：采用胶束电动色谱(MEKC)法对血塞通滴丸中5种皂苷类成分进行含量测定,建立MEKC指纹图谱并结合相似度分析对产品进行批次质量一致性评价。以20 mmol·L^(-1)硼砂-20 mmol·L^(-1)硼酸(pH 8.5)、55 mmol·L^(-1)十二烷基硫酸钠(SDS)、23 mmol·L^(-1)β-环糊精、13%异丙醇作为运行缓冲液,分离电压20 kV,检测波长203 nm,采用75μm×50.2 cm(有效长度40.0 cm)的毛细管柱,在25℃下进行分析。对三七皂苷R1和人参皂苷Rg_(1)、Re、Rb_(1)、Rd进行含量测定,设定各成分质量控制范围;并建立血塞通滴丸的指纹图谱,通过相似度分析评价血塞通滴丸的批次一致性。19批血塞通滴丸中5种皂苷类成分在一定范围内保持稳定,对多批次样品分析数据进行统计分析,建议其质量控制范围设定为三七皂苷R121.92~34.16 mg·g^(-1),人参皂苷Rg183.54~131.78 mg·g^(-1),人参皂苷Re 13.58~19.82 mg·g^(-1),人参皂苷Rb189.40~129.90 mg·g^(-1),人参皂苷Rd 22.34~35.67 mg·g^(-1)。建立的指纹图谱共标定11个共有峰,通过标准对照品比对鉴定出三七皂苷R1,人参皂苷Rg1、Re、Rb1和Rd等5个共有峰;所有批次样品的相似度在0.988以上,质量批次一致性较好。该方法绿色环保、快捷方便,可用于血塞通滴丸含量测定及质量评价,并可为其他中药滴丸制剂的质量控制提供参考。The present study determined five saponins in Xuesaitong Dropping Pills(XDP)by micellar electrokinetic chromatography(MEKC),and evaluated between-batch consistency by MEKC fingerprints and similarity analysis.A background buffer was composed of 20 mmol·L^(-1) sodium tetraborate-20 mmol·L^(-1) boric acid solution(pH 8.5),55 mmol·L^(-1) sodium dodecyl sulfate(SDS),23 mmol·L^(-1)β-cyclodextrin,and 13%isopropyl alcohol.All separations were performed at 25℃,20 kV and the detection wavelength was set at 203 nm.The separation channel was a fused silica capillary with a dimension of 75μm I.D.and a total length of 50.2 cm(effective length of 40.0 cm).The contents of notoginsenoside R_(1),and ginsenosides Rg1,Re,Rb1,Rd were determined with their quality control ranges set.The fingerprints of XDP were established and the between-batch consistency was evaluated by similarity analysis.The contents of five saponins from the 19 batches of XDP were stable in the fixed ranges.Statistical analysis was carried out on the results of multiple batches of samples,and the specific quality control ranges were recommended as follows:notoginsenoside R121.92-34.16 mg·g^(-1),ginsenosides Rg183.54-131.78 mg·g^(-1),ginsenosides Re 13.58-19.82 mg·g^(-1),ginsenosides Rb189.40-129.90 mg·g^(-1),and ginsenosides Rd 22.34-35.67 mg·g^(-1).Eleven characteristic peaks were identified in the fingerprints.Five peaks,notoginsenoside R1 and ginsenosides Rg1,Re,Rb1,Rd,were identified with reference standards.The similarities of the 19 batches of samples were all above 0.988,indicating good between-batch consistency.This method is green and simple,and can be used for the quantitative determination and quality evaluation of XDP.It can also provide references for the quality control of other Chinese medicinal dripping pills.

关 键 词：血塞通滴丸 胶束电动色谱 指纹图谱 质量一致性评价 

分 类 号：R286.0[医药卫生—中药学]