清开灵滴丸质量控制方法的优化研究  

Optimization of the Quality Control Method of Qingkailing Dropping Pills

作　　者：闫海霞[1] 傅欣彤[1] 陈有根[1] 郭洪祝[1] 常增荣[1] YAN Hai-xia;FU Xin-tong;CHEN You-gen;GUO Hong-zhu;CHANG Zeng-rong(Beijing Center for Health Food and Cosmetics Control,Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine,Beijing Institute for Drug Control,Beijing 102206,China)

机构地区：[1]北京市药品检验所,北京市保健食品化妆品检验中心,中药成分分析与生物评价北京市重点实验室,北京102206

出　　处：《中国药学杂志》2020年第6期465-472,共8页Chinese Pharmaceutical Journal

基　　金：国家药品标准提高暨2020年版药典科研项目资助。

摘　　要：目的优化并完善清开灵滴丸的质量控制方法。方法采用高效液相色谱法对清开灵滴丸中的黄芩苷进行鉴别;采用薄层色谱法对清开灵滴丸中金银花及其所含绿原酸、栀子所含栀子苷进行鉴别。采用高效液相色谱法-蒸发光检测器同时测定清开灵滴丸中胆酸和猪去氧胆酸的含量,色谱柱为Phenomenex Gemini 110 C18(4.6 mm×250 mm,5μm),流动相为甲醇-乙腈-0.1%甲酸(68:17:15),流速为1.0 mL·min^-1。采用高效液相色谱法测定清开灵滴丸中扼子苷的含量,色谱柱为Agilent Eclipse XDB-C18(4.6 mm×150 mm,5μm);流动相为乙腈-0.05%磷酸(10:90),流速为1.0 mL·min^-1;检测波长为238 nm。采用高效液相色谱法测定清开灵滴丸中黄芩苷的含量,色谱柱为同栀子苷含量测定;流动相为甲醇-水-鱗酸(47:53:0.2),流速为1.0 mL·min^-1;检测波长为Z75 nmD结果薄层色谱斑点清晰,重现性好。猪去氧胆酸、胆酸、栀子苷和黄芩苷进样量分别在0.5050?6.312μg、0.515?6.440μg、0.02912?0.5824μg和0.1092?1.092μg内与冷面积(或峰面积对数)呈良好线性关系,平均回收率分别为101.5%、101.6%、98.61%和99.77%,RSD分别为1.7%、1.5%、1.42%和0.79%。结论提高后的质量标准分析方法简便、快速、准确且毒性较小,能更全面有效控制清开灵滴丸的质量。OBJECTIVE To optimize and improve the quality standard of Qingkailing dropping pills.METHODS Lonicerae Japonicae Flos,geniposide in Gardeniae Fructus and baicalin in Scutellariae Radix of Qingkailing dropping pills were identified by TLC and HPLG respectively.Cholic acid and hydrodeoxycholic acid were determined by HPLC equipped with an ELSD and a column(4.6 mm×250 mm,5μm)packed with ODS bonded silica gel(5μm particle size).The mobile phase was a mixture of methanol,acetonitrile and 0.1%formic acid(68:17:15,V/V/V)and the flow rate was 1.0 mL·min^-1.Geniposide in Gardeniae Fructus of Qingkailing dropping pills was determined by HPLC equipped with a DAD(238 nm)and a column(4.6 mm×250 mm)packed with ODS bonded silica gel(5μm particle size).The mobile phase was a mixture of acetonitrile and 0.05%phosphoric acid(10:90,V/V)and the flow rate was 1.0 mL·min^-1.Baicalin in Scutellariae Radix of Qingkailing dropping pills was determined by HPLC e-quipped with a DAD(275 nm)and a column(4.6 mm×150 mm)packed with ODS bonded silica gel(5μm particle size),the mobile phase was a mixture of methnol,water and phosphoric acid(47:53:0.2,V/V/V),and the flow rate was 1.0 mL·min^-1.RESULTS The developed TLC spots were clear with good reproducibility.Hydrodeoxycholic acid,cholic acid,geniposide and baicalin showed good linear relationship in the ranges of 0.5050-6.312μ,0.515-6.440μg,0.02912-0.5824μg,and 0.1092-1.092μg,respectively.The average recoveries(n=6)were 101.5%,101.6%,98.61%and 99.77%,with RSDs of 1.7%,1.5%,1.42%and 0.79%,respectively.CONCLUSION The method is simple,rapid,accurate,with low toxicity,and can be used to control the quality of Qingkailing dropping pills more effectively and comprehensively.

关 键 词：清开灵滴丸 胆酸 猪去氧胆酸 金银花 栀子苷 黄芩苷 薄层色谱 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]