顶空气相色谱法测定大孔树脂提取物中的残留溶剂研究  

Determination of residual solvents in macroporous resin extracts by Head-space capillary gas chromatography

作　　者：刘冬[1,2] 杨敬芝[2] 杜守颖[1] 张东明[2] 赵立敏[2] 陈雯[1] 

机构地区：[1]北京中医药大学中药学院,北京100102 [2]中国医学科学院药物研究所,北京100050

出　　处：《药物分析杂志》2009年第11期1877-1880,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立了测定大孔树脂淫羊藿提取物、栀子提取物以及HP中乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯残留有机溶剂含量的顶空气相色谱法。方法:采用顶空气相色谱法,FID检测器,以20%～50%二甲基亚砜为溶媒,顶空预热温度为90℃,预热时间为10 min,进样口温度为180℃,检测器温度为250℃,以氮气为载气,使用DB-1交联毛细管柱(60m×0.32mm,1μm),程序升温,实现了各组分的基线分离。结果:乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯在各自对应的浓度范围内,线性关系良好;乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯的最小检测限分别为2.72,0.22,0.03,0.03,0.28,0.33,0.03,0.31μg.mL-1;加样回收率均在75%以上,精密度较好。结论:经方法学验证,该方法灵敏、准确、可靠,可适用于大孔树脂淫羊藿提取物、栀子提取物及HP中乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯等残留有机溶剂的测定。Objective： This paper reports a Head-space GC method for determination of enthanol, hexane, benzene,toluene, methyl cyclohexane ,xylene, styrene, divinyl benzene in macroporous resin extractions. Method： The analytical column was DB-1（60m×0.32mm,1μm）.The injector temperature was 180 ℃ and the detector temperature was 250℃. The column temperature was programmed raised. The carrier gas was nitrogen and the solvent was 20%–50% dimethyl sulfoxide. Results： The stand curve were linear for each solvents in the range of each consistency. The average recoveries were all more than 75%. Conclusion： This method is simple, rapid and precise, it is suitable for measurement of residual solvents in macroporous resin extracts.

关 键 词：顶空进样法 毛细管气相色谱法 淫羊藿提取物 栀子提取物 HP 溶剂残留测定 

分 类 号：R917[医药卫生—药物分析学]