高效液相色谱-蒸发光散射检测法测定中乌宁碱的含量

Determination of Mesaconine by HPLC-ELSD Method

目的建立高效液相色谱-蒸发光散射检测法（HPLC—ELSD）测定中乌宁碱的含量。方法使用Gemini C18 110A（4．6mm×150mm，5μm）色谱柱，以甲醇-0．1％三氟乙酸（25：75）为流动相，流速为0．6mL·min^-1，使用Alhech ELSD 2000ES检测器，漂移管温度90℃，气体流速2．3L·min^-1。结果中乌宁碱在0．40～0．60mg·mL^-1内峰面积的对数与浓度的对数呈良好线性关系（r=0．9996）；进样精密度RSD为0．04％（n=5）；重复性试验RSD为0．7％（n=6）；日内精密度RSD为0．4％；日间精密度RSD为0．6％；平均回收率为101．0％（RSD=1．1％；n=9）。结论本法专属、简便、准确，适用于中乌宁碱的含量测定。

OBJECTIVE To establish an HPLC-ELSD method for determination of mesaconine. METHODS Gemini C 18 110A column （4.6mm×150mm,5μm） was adopted with the mobile phase consisting of methanol-0. 1% TFA （25： 75 ） at the flow rate of 0. 6 mL·min^-1. The detector was Alltech ELSD 2000ES, with the drift tube temperature of 90 ℃ and the airflow velocity of 2. 3 L·min^-1. RESULTS Under this conditions, mesaconine and the related substances were well separated. The linear range of mesaco- nine was 0. 40 -0. 60 mg·mL^-1 （r =0. 999 6）. RSD of injection precision and repeatability test were 0. 04% （n =5） and 0. 7% （n = 6 ） , the intra day and inter day precision RSD were 0. 4% and 0. 6% , respectively. The average recovery was 101.0% （RSD = 1.1% , n = 9）. CONCLUSION The established method was specific, simple, accurate, and suitable for determination of mesaconine.