浙江中西医结合杂志

张志坚,杨兆丽,张加颂,刘澎,谢丹娥,王琪.HPLC法测定青蒿素哌喹片中哌喹有关物质[J].浙江中西医结合杂志,2019,29(10):

HPLC法测定青蒿素哌喹片中哌喹有关物质

Determination of piperaquine-related substances in artemisinin piperaquine tablets by HPLC

投稿时间：2019-04-23 修订日期：2019-07-30

DOI：

英文关键词:Artemisinin piperaquine tablets piperaquine HPLC Related substances

基金项目:“扬帆计划”引进创新创业团队专项资助；国家“重大新药创制”科技重大专项；广州市科技计划

作者	单位	E-mail
张志坚	广东新南方青蒿药业股份有限公司，广东新南方青蒿科技有限公司	zhangzj@xnfyy.com
杨兆丽^*	广东新南方青蒿药业股份有限公司，广东新南方青蒿科技有限公司	5210340@qq.com
张加颂	广东新南方青蒿药业股份有限公司
刘澎	广东新南方青蒿药业股份有限公司
谢丹娥	广东新南方青蒿药业股份有限公司
王琪	广州中医药大学科技产业园有限公司

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中文摘要:

【目的】采用HPLC法对青蒿素哌喹片中哌喹的有关物质进行检查。【方法】色谱柱为Thermo BDS HYPERSIL C18（250*4.6 mm，5 μm），流动相为乙腈：0.1%三氯乙酸：三乙胺（18:82:0.2，磷酸调pH至2.5），流速1.0 mL?min-1，柱温为25 ℃，检测波长为349 nm。【结果】哌喹杂质Ⅰ 0.0102～8.1800 μg?mL-1与峰面积的线性关系良好（R2=1.0000），加样回收率为94.5%~96.9%，RSD为2.0%（n=9），定量限为0.01 μg?mL-1，检测限为0.002 μg?mL-1；杂质Ⅱ 0.0205～8.1800 μg?mL-1与峰面积的线性关系良好（R2=0.9999），加样回收率为90.8%~100.4%，RSD为4.8%（n=9），定量限为0.02 μg?mL-1，检测限为0.004 μg?mL-1；杂质Ⅲ 0.0597～7.9600 μg?mL-1与峰面积的线性关系良好（R2=1.0000），加样回收率93.4%~98.7%，RSD为3.6%（n=9），定量限为0.06 μg?mL-1，检测限为0.021 μg?mL-1。【结论】该方法专属性强、准确、灵敏，适用于青蒿素哌喹片中哌喹的有关物质检查。

英文摘要:

Objective To detect the piperaquine-related substances in artemisinin piperaquine tablets by HPLC. Methods Thermo BDS HYPERSIL C18（250*4.6mm，5 μm）column was used with UV detection at 349 nm,and the mobile phase consisted of acetonitrile and 0.1% trichloroacetate and triethylamine (18:82:0.2, adjusted pH to 2.5 with phosphoric acid).The flow rate was 1.0mL?min-1,The column temperature was 25 ℃. Results The calibration curve was linear （R2=1.0000） within the range of 0.0102～8.1800 μg?mL-1 for piperaquine impurityⅠ. The sample recovery was 94.5%~96.9%，with RSD=2.0%（n=9）.The quantitative limit was 0.01 μg?mL-1 and the detection limit was 0.002 μg?mL-1; The calibration curve was linear （R2=0.9999） within the range of 0.0205～8.1800 μg?mL-1 for impurity Ⅱ. The sample recovery was 90.8%~100.4%，with RSD=4.8%（n=9）.The quantitative limit was 0.02 μg?mL-1 and the detection limit was 0.004 μg?mL-1; The calibration curve was linear （R2=1.0000） within the range of 0.0597～7.9600 μg?mL-1 for impurity Ⅲ. The sample recovery was 93.4%~98.7%，with RSD=3.6%（n=9）.The quantitative limit was 0.06 μg?mL-1 and the detection limit was 0.021 μg?mL-1. Conclusion The method is specific,accurate and sensitive,and is suitable for the detection of artemisinin-related substances in artemisinin piperaquine tablets.

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