HPLC法测定青蒿素哌喹片中青蒿素有关物质  

Determination of Artemisinin-related Substances in Artemisinin Piperaquine Tablets by HPLC

作　　者：张志坚 杨兆丽 谢丹娥 刘澎 张加颂 宋健平[3] ZHANG Zhi-Jian;YANG Zhao-Li;XIE Dan-E;LIU Peng;ZHANG Jia-Song;SONG Jian-Ping(ArtephamiCo., Ltd., China, Meizhou 514300 Guangdong, China;ARTEPHARM CO., LTD., CHINA, Meizhou 514300Guangdong, China;Guangzhou University of Chinese Medicine, Guangzhou 510405 Guangdong, China)

机构地区：[1]广东新南方青蒿药业股份有限公司,广东梅州514300 [2]广东新南方青蒿科技有限公司,广东梅州514300 [3]广州中医药大学,广东广州510405

出　　处：《广州中医药大学学报》2019年第10期1611-1617,共7页Journal of Guangzhou University of Traditional Chinese Medicine

基　　金：国家“重大新药创制”科技重大专项（编号：2018ZX09303-008）;国家自然科学基金资助项目（编号：81873218）;“扬帆计划”引进创新创业团队专项资助（编号：2014YT02S008）

摘　　要：【目的】采用高效液相色谱(HPLC)法建立检测青蒿素哌喹片中青蒿素有关物质的方法。【方法】色谱柱为YMC-Triart C18(250 mm×4.6 mm,5μm),流动相为乙腈-0.01%三氯乙酸(V∶V=50∶50),流速为1.0 m L/min,柱温为35℃,检测波长为210 nm。【结果】青蒿素15~51μg/mL与峰面积的线性关系良好(r=0.999 4),定量限为15μg/mL,检测限为5μg/mL。杂质A(青蒿烯)0.3~30μg/mL与峰面积的线性关系良好(r=0.999 9),加样回收率为95.08%~98.06%,相对标准偏差(RSD,s R)为1.04%(n=12),定量限为0.25μg/mL,检测限为0.075μg/mL。杂质B(9-epi-Artemisinin)10~46μg/mL与峰面积的线性关系良好(r=0.998 1),加样回收率82.10%~89.65%,s R为3.21%(n=9),定量限为10μg/mL,检测限为3μg/mL。【结论】该方法专属性强、准确、灵敏,适用于青蒿素哌喹片中青蒿素的有关物质检测。Objective To establish a method for detecting artemisinin-related substances in Artemisinin Piperaquine Tablets by high performance liquid chromatography(HPLC). Methods HPLC was performed on YMCTriart C18(250 mm × 4.6 mm,5 μm)with mobile phase consisting of acetonitrile and 0.01% trichloroacetate(V∶V = 50∶50). The flow rate was 1.0 m L/min,column temperature was 35 ℃,and detection wave was 210 nm.Results There was a good linear relationship for artemisinin within the range of 15~51 μg/mL with the peak area(r =0.999 4). The quantitative limit was 15 μg/mL, and detection limit was 5 μg/mL. There was a good linear relationship for impurity A(artemisitene)within the range of 0.3~30 μg/mL with the peak area(r = 0.999 9),the sample recovery was 95.08%~98.06%, s R = 1.04%(n = 12), the quantitative limit was 0.25 μg/mL, and detection limit was 0.075 μg/mL. There was a good linear relationship for impurity B(9-epi-Artemisinin)within the range of 10~46 μg/mL with the peak area(r = 0.998 1),the sample recovery was 82.10%~89.65%,s R =3.21%(n = 9),the quantitative limit was 10 μg/mL,and detection limit was 3 μg/mL. Conclusion The method is specific,accurate and sensitive,and suitable for the detection of artemisinin-related substances in Artemisinin Piperaquine Tablets.

关 键 词：青蒿素哌喹片 青蒿素 HPLC 

分 类 号：R284.1[医药卫生—中药学]