高效液相色谱法检测血清中的高三尖杉酯碱

目的：利用高效液相色谱法测定血清中的高三尖杉酯碱的含量。方法：以内标法为基础，取１ｍＬ血清标本加入内标三尖杉酯碱，经二氯甲烷２次重复提取，减压蒸干，残渣用流动相溶解，进样。色谱条件：以Ｃ１８反相柱为分析柱，流动相组成为０１ｍｏｌ·Ｌ－１甲酸铵－甲醇（２∶１），流速为１０ｍＬ·ｍｉｎ－１，在紫外检测器波长２９０ｎｍ处进行检测。结果：方法学检查：最低检测限２ｎｇ·ｍＬ－１，在４～１５００ｎｇ·ｍＬ－１范围内呈线性，回收率９１３％（ｎ＝８），批内和批间的相对标准偏差分别为１２％（ｎ＝８）和３６％（ｎ＝４）。结论：对临床化疗常与之配伍使用的３种药物，进行干扰实验，未发现干扰峰。

Determination of the Content of Homoharringtonine in Serum by HPLC

Objective: Determination of the content of homoharringtonine(HHT)in Serum by HPLC is reported. Method: On the basis of internal standard method,10 mL serum sample was extracted by CH2Cl2 two times. The organic phase was evaporated by HBI vortex evaporator.The residue was dissolved in mobile phase and injected to HPLC. The C18 reversedphase column was used, mobile phase:methanol-01 molL-1 ammonium formate (12),flow rate 10 mLmin-1 and harringtonine(HT) as internal standard.The detection was carried out with an ultraviolet detector (=290 nm ). Results: The detection limit of HHT was 4 ngmL-1. The linearity was in the range of 41 500 ngmL-1.The absolute recovery of HHT and HT was respectively 9125%(n=8) and 9275%(n=4).The betweenday RSD HHT was 123%(n=8), and intraday RSD was 355%(n=4)respectively. Conclusion: We did not find any interference peak from three commonly drugs(ADR,DNR and AraC) used in combination therapy.