顶空-气相色谱法测定绞股蓝总苷中的溶剂残留  

Determination of residual solvents in gypenosides by headspace capillary GC

作　　者：骆文婷 刘雪峰 李霞 绳金房 刘海静[1,2] LUO Wen-ting;LIU Xue-feng;LI Xia;SHENG Jin-fang;LIU Hai-jing(Shaanxi University of Chinese Medicine,Xianyang 712046,China;Shaanxi Institute for Food and Drug Control,Xi’an 710065,China)

机构地区：[1]陕西中医药大学,咸阳712046 [2]陕西省食品药品监督检验研究院,西安710065

出　　处：《药物分析杂志》2020年第3期488-494,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：陕西省科技厅中药特色产业创新链(群)项目(2019TSLSF01-01)。

摘　　要：目的:建立顶空-气相色谱法测定绞股蓝总苷原料药中8种残留溶剂的分析方法。方法:采用顶空-毛细管气相色谱法,DB-WAX毛细管色谱柱(30 m×0.32 mm,0.25μm),氢火焰离子化检测器,载气为氮气,流速1.5 mL·min-1;柱温为程序升温,进样口温度为220℃,检测器温度为250℃。顶空进样,顶空平衡温度100℃,平衡时间为30 min,定量环温度105℃,传输管温度110℃,进样量1 mL,低速振摇。结果:测定的8种有机溶剂完全分离,线性关系良好。苯、甲苯、二甲苯、二乙烯苯、苯乙烯、甲醇、乙醇和正丁醇的平均回收率分别为96.9%、98.4%、96.6%、99.5%、96.8%、99.7%、98.4%和98.7%。8批样品中有6批的有机溶剂残留量均在规定的范围内,2批正丁醇和二乙烯苯残留量高于限度。结论:本方法可以较好地用于测定绞股蓝总苷中的残留溶剂。Objective:To establish a GC method for the determination of residual solvents in gypenosides. Methods:The residual solvents in gypenosides were separated and detected by DB-WAX capillary column(30 m×0.32 mm,0.25 μm)with FID detector. The carried gas was nitrogen,and the gas flow rate was 1.5 mL·min-1.The column temperature was programmed. The inlet temperature was 220 ℃ and FID detector temperature was set at 250 ℃.The split ratio was 10∶1. Headspace conditions were as follows:the temperature and the time of balance for the sample were 100 ℃ and 30 min;the temperature of quantitative loop and transfer lines was 105 ℃ and 110 ℃,respectively.The sample volume was 1 mL,with low-speed shaking. Results:The 8 residual solvents tested were completely separated and the linear relationship was good. The average recoveries for benzene,toluene,xylene,divinylbenzene,styrene,methanol,ethanol and n-butanol were 96.9%,98.4%,96.6%,99.5%,96.8%,99.7%,98.1% and 98.7%,respectively. The residual amount of organic solvents in 6 batches was within the specified range,and the residual amount of 2 batches for n-butanol and divinylbenzene was above the limit. Conclusion:This method can be used to determine the residual solvents in gypenosides.

关 键 词：绞股蓝总苷 气相色谱 残留溶剂 顶空进样 大孔树脂 

分 类 号：R917[医药卫生—药物分析学]