顶空进样气相色谱法测定葛根提取物中有机溶剂残留研究

目的探讨测定葛根提取物中有机溶剂残留的方法。方法用顶空进样气相色谱法【色谱柱：HP-Innowax（30．00mm×0．32mm，0．25μm）石英毛细管柱；载气：氮气；流速：0．8mL／min；进样器温度：200℃；检测器类型及温度：氢焰离子化检测器（FID），220℃；柱升温程序：50℃保持10min，然后以20℃／min的速度升至190℃，保持3min；顶空条件平衡温度：85℃；平衡时间：15min；传输管温度：105oc；进样环温度：125℃。】测定葛根提取物中有机溶剂的残留．将各有机溶剂对照按照限度制成混合对照品，样品中相应位置的峰值应不高于对照溶液，并对参数进行验证。结果正己烷、乙醇、苯、甲苯、乙苯、对二甲苯、间二甲苯、正丁醇、邻二甲苯、苯乙烯、对二甲苯、二乙烯苯分别在1．99-59．72、2．00～59．87、0．38-11．33、1．98。59．43、1．98～59．39、1．98—59．47、1．97～59．07、1．97～59．20、1．98-59．45、1．99-59．74、1．99~59．59、1．98～59．26txg／mL内，其峰面积与浓度呈良好的线性关系，R。值均在0．9990以上，精密度、回收率均符合要求，空白溶剂对样品的测定没有影响，3批样品检验均符合限度要求。结论顶空进样气相色谱法测定葛根提取物中有机溶剂，方法简单、结果准确。

Study of gas chronatography-headspace injection method for the determination of residual organic solvent in extracts from pueraria

Objective To explore the method for the determination of residual organic solvent in extracts from pueraria. Methods Gas chromatography（GC）-headspaee injection method was adopted to measure the residual organic solvent in extracts from pueraria. The HP-Innowax （30.00 mm×0.32mm,0.25μm）quartz capillary column was used as chromatographic column;the nitrogen gas was used as carrier gas at a flow rate of 0.8 mL/min; the injector temperature was 200 ℃ ;the detector was flame ion- ization detector（FID） with the temperature of 220 ℃ ; the temperature program comprised two phases ： initially the temperature was set at 50 ℃ for 10 min,and then ramped to 190 ℃ at a rate of 20 ℃/min and held for 14 min;the equilibrium temperature of headspace was 85 ℃ ;the equilibrium time was 15 min;the capillary temperature was 105 ℃ ,and the injection ring temperature was 125 ℃. The organic solvent was mixed with each limitation as contrast solution, and the corresponding position in the sample peak should not be higher than that in the contrast solution. The parameters were verified. Results When the density of n-hexane was between 1.99-59.72 μg/mL,ethyl alcohol between 2.00-59.87 μg/mL,benzene between 0.38-11.33 μg/mL,methylbenzene between 1.98 -59.43 μg/mL, ethylbenzene between 1.98 -59.39 g/mL, p-xylene between 1.98 -59.47 μg/mL, m-Xylene between 1.97-59.07μg/mL,n-butyl alcohol between 1.97-59.20 μg/mL, o-xylene between 1.98-59.45 μg/mL, phenylethylene between 1.99-59.74 μg/mL, p-xylene between 1.99-59.59 μg/mL and divinylbenzene between 1.98-59.26 μg/mL respectively,its peak areas had good linear relationship with its concentration, and the average R2 were all above 0.999. The precision and recovery rate of the method meet the requirements, and the blank solvent had no affect. Three samples are all accordance with the requirement after examination. Conclusion Headspaee injection method for the determination of residual organic solvent in extracts from pueraria is simple and reliable.