摘要：
目的:建立顶空-气相色谱法测定人参总皂苷中10种树脂残留成分的含量.方法:以10％的N,N-二甲基甲酰胺为提取溶剂,采用顶空进样,毛细管柱气相色谱测定树脂残留成分.柱温为程序升温(起始温度为60°C,保持1 min,以0.3°C·min-1升至62°C,再以10°C·min-1升至140°C,保持5 min);进样口温度:220°C,检测器温度:250°C.FID检测器,载气为氮气,流速1 mL· min-1,分流比为10∶1;项空进样,顶空平衡温度90°C,平衡时间为30 min,定量环温度110°C,传输管温度130°C,进样量1 mL,低速振摇.结果:10种有机溶剂残留物的峰面积与质浓度呈良好线性关系,正己烷、甲基环己烷、苯、甲苯、对二甲苯、间二甲苯、邻二甲苯、苯乙烯、1,2-二乙基苯和二乙烯苯的平均回收率分别为102.65％、100.96％、103.34％、104.69％、96.14％、96.83％、96.81％、103.78％、94.69％和102.64％,3批市售样品除检出残留物邻二甲苯(含量分别为1.51、1.18、1.48 μg· g-1)外,其他9种残留成分未检出.结论:所建立的方法能够较好地对人参总皂苷中10种树脂残留物进行限度测定.%Objective:To develop a determination method of ten resin residues in total saponins of Panax Ginseng by headspace GC.Method:The sample was dissolved with 10％ DMF and analyzed by headspace capillary gas chromatography.The temperature program for the column was as follows:initially heated at 60 °C for 1 min,rose to 62 °C at a speed of 0.3 °C · min-1;then rose to 140 °C at a speed of 10 °C · min-1,lasting for 5 min.The inlet temperature was 220 °C and FID detector temperature was set at 250 °C.The split ratio was 10 ∶ 1 and the flow rate of the carrier gas (N2) was 1 mL · min-1.Headspace conditions were as follows:the temperature and the time of balance for the sample were 90 °C and 30 min;the temperature of quantitative loop and transfer lines was 110 °C and 130 °C.The sample volume was 1 mL,with low-speed shaking.Result:Linear relations between peak area and concentration of ten residues were good,average recoveries of n-hexane,hexahydrotoluene,benzene,methylbenzene,p-xylene,m-xylene,o-xylene,styrene,1,2-diethylbenzene and divinylbenzene were 102.65％,100.96％,103.34％,104.69％,96.14％,96.83％,96.81％,103.78％,94.69％ and 102.64％,respectively.O-xylene was detected in three batches of samples from market(the content was 1.51,1.18 and 1.48 μtg· g-1,respectively),and the other nine residues were not found in the samples.Conclusion:The method was suitable for detecting ten resin residues in total saponins of Panax Ginseng.
