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

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.