一次萃取后正相HPLC法定量测定维生素AD微丸的含量  

One-step Extraction Followed by Normal Phase HPLC for Quantitative Analysis of Vitamin AD Micropellets

作　　者：周远华[1] 张立雯[1] 董顺玲[1] ZHOU Yuanhua;ZHANG Liwen;DONG Shunling(Guangzhou Institute for Drug Control,Guangzhou 510160)

机构地区：[1]广州市药品检验所,广东广州510160

出　　处：《中国医药工业杂志》2022年第6期890-895,共6页Chinese Journal of Pharmaceuticals

摘　　要：建立了正相HPLC法测定维生素AD微丸(1)中全反式维生素A棕榈酸酯(2)和维生素D(3)的含量,前处理只需采用正己烷萃取1次。色谱柱采用Phenomenex Luna NH100A柱(4.6 mm×250 mm,3μm),流动相为正己烷,检测波长为265 nm。结果显示,全反式2和3分别在329.4~1647.1和19.23~192.3 IU/ml内线性关系良好;重复性试验RSD(n=6)分别为0.6%和0.5%,检测限分别为0.015、0.28 IU/ml;平均回收率(n=9)分别为100.7%和99.3%,RSD分别为1.9%和0.9%。建立的萃取方法能够一次性、完全地提取1中的全反式2和3;分析方法能够准确测定2和3,专属性强、灵敏度高,为1的质量控制提供了参考。A normal phase HPLC method was established for the determination of all-trans vitamin A palmitate(2)and vitamin D(3)in vitamin AD micropellets(1),and the pretreatment only required one-step extraction with n-hexane.A Phenomenex Luna NH100A column(4.6 mm×250 mm,3μm)was used,with the mobile phase of n-hexane,and the detection wavelength was 265 nm.The results showed that it was linear for all-trans 2 and 3 in the ranges of 329.4-1647.1 and 19.23-192.3 IU/ml,respectively.The repeatability RSDs of all-trans 2 and 3(n=6)were 0.6%and 0.5%,and the detection limits were 0.015 and 0.28 IU/ml,respectively.The mean recoveries(n=9)of all-trans 2 and 3 were 100.7%and 99.3%,with the RSDs of 1.9%and 0.9%,respectively.The extraction method could completely extract all-trans 2 and 3 from 1 in one-step,and the determination method could accurately determine the contents of all-trans 2 and 3 with high specificity and sensitivity,which provided a reference for the quality control of 1.

关 键 词：一次萃取 维生素AD微丸 正相高效液相色谱法 含量测定 

分 类 号：R917[医药卫生—药物分析学]