摘要
目的:建立超高效液相色谱串联三重四极杆质谱测定注射用银杏叶提取物及其制剂中总银杏酸的方法。方法:采用HLB固相萃取净化制剂,Waters Cortecs T3色谱柱(50 mm×2. 1 mm,2. 7μm),以甲醇-1%冰醋酸溶液(90∶10)为流动相,在电喷雾离子化负离子模式下,以多反应监测方式(MRM)检测。结果:银杏酸C13:0、C15:1、C17:1在0～50 ng/mL范围内成良好线性关系,相关系数均大于0. 999;平均加样回收率为97. 3%～115. 2%,相对标准偏差(RSD)为0. 3%～3. 4%;检出限分别为0. 03、0. 06、0. 04 mg/kg。结论:本方法可应用于实际样品的测定。
Objective: To develop an analytical method for determination of ginkgolic acids in the ginkgo biloba extract for injection and its preparation by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry. Methods: The preparations were purified by HLB SPE.A chromatographic column,Waters Cortecs T3(50 mm×2.1 mm,2.7 μm),was used with methanol-1% acetic acid(90∶ 10)as the mobile phase.The ginkgo acids were detected by electrospray ionization mass spectrometry in negative mode with multiple reaction monitoring(MRM)mode. Results: Ginkgo Acid C13:0,C15:1 and C17:1 possessed good linear correlation in the mass concentration range from 0 to 50 ng/mL,with the correlation coefficients more than 0.999.The mean recoveries were in the range of 97.3%-115.2%,and the RSDs were 0.3%-3.4%.The limits of quantification were 0.03,0.06,0.04 mg/kg,respectively. Conclusion: The method could be applied to the analysis of ginkgolic acids in actual samples.
作者
孙健
李丽敏
胡青
诸艳蓉
毛秀红
季申
Sun Jian;Li Limin;Hu Qing;Zhu Yanrong;Mao Xiuhong;Ji Shen(Shanghai Institute for Food and Drug Control,Shanghai 201203,China)
出处
《世界中医药》
CAS
2019年第4期818-821,共4页
World Chinese Medicine
基金
上海市科学技术委员会基金项目(18DZ2292200)
