Wang Han, Tang Yizhu, Zhao Xiaoya, Ye Cheng, Guo Shaofei, Luo Jing, Xiong Lu, Cao Wei, Wu Jian'an, Wang Peng
Technology Center of Wuhan Customs, Wuhan 430050, Hubei.
Hubei Institute of Sport Science, Wuhan 430205, Hubei.
Se Pu. 2019 Oct 8;37(10):1036-1041. doi: 10.3724/SP.J.1123.2019.01055.
A method combining QuEChERS with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of higenamine in Chinese herbal medicine, condiments, and topical medicine. The sample was subjected to extraction using a formic acid-ethanol mixture, followed by purification of the QuEChERS sorbents; then, the extraction solution was introduced into the LC-MS/MS system for detection in multiple reaction monitoring (MRM) mode. Under the optimal conditions, the detection limit of the developed method was 0.03 ng/g, and the linear range was 0.10-100 ng/g with a relative standard deviation (RSD) of 4.33% (0.5 ng/g, =7). The method was then applied to the determination of higenamine in 13 kinds of Chinese herbal medicine, four kinds of condiments, and a topical medicine. Higenamine was detected in dried lotus leaf, dried lotus seed, Chinese yam, Yuzhu, Yam, Sichuan pepper, Cassia, and the topical medicine at 9667.6, 1183.8, 21.5, 8.2, 8.5, 148.6, 21.3, and 173.3 μg/kg, respectively. The recoveries of higenamine in Sichuan pepper and cassia was 92.6%-109.8%. In conclusion, the method is fast, simple, reliable, and suitable for use in batch operation.
建立了一种将QuEChERS与液相色谱 - 串联质谱法(LC-MS/MS)相结合的方法,用于测定中药材、调味品和外用药中的去甲乌药碱。样品先用甲酸 - 乙醇混合物进行萃取,然后用QuEChERS吸附剂进行净化;接着,将萃取液引入LC-MS/MS系统,以多反应监测(MRM)模式进行检测。在最佳条件下,所建立方法的检出限为0.03 ng/g,线性范围为0.10 - 100 ng/g,相对标准偏差(RSD)为4.33%(0.5 ng/g,n = 7)。该方法随后应用于13种中药材、4种调味品和1种外用药中去甲乌药碱的测定。在干荷叶、干莲子、山药、玉竹、山药、花椒、肉桂和外用药中分别检测到去甲乌药碱,含量分别为9667.6、1183.8、21.5、8.2、8.5、148.6、21.3和173.3 μg/kg。花椒和肉桂中去甲乌药碱的回收率为92.6% - 109.8%。综上所述,该方法快速、简便、可靠,适用于批量操作。