气相色谱法测定6种中药提取物中大孔吸附树脂有机残留物  

Determination of the Residua from Macroporous Resin in Traditional Chinese Medicine Extract by GC

作　　者：王少敏[1] 钱大公[1] 王柯[1] 季申[1] 

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《中国药学杂志》2009年第1期55-58,共4页Chinese Pharmaceutical Journal

摘　　要：目的建立测定6种中药提取物中正已烷、苯、甲苯、对二甲苯、邻二甲苯、苯乙烯、1，2-二乙基苯和二乙烯苯共8种大孔吸附树脂有机残留物的方法。方法以聚乙二醇为固定相的毛细管色谱柱，氢火焰离子检测器，顶空进样方式，柱温：起始温度为60℃，程序升温起始温度为60℃，保持16min，以每分钟20℃的升温速率升至200℃，保持2min。结果8种成分分离良好，均有良好的线性范围，分别为正己烷1．386-46．2μg（r=0．9975），苯0．4749-15．83μg（r=0．9996），甲苯1．488-49．6μg（r=0．9993），对二甲苯1．4778-49．26μg（r=0．9991），邻二甲苯1．8183-60．61μg（r=0．9990），苯乙烯1．5474-51．58μg（r=0．9995），1，2-二乙基苯1．6206-54．02μg（r=0．9981）和二乙烯苯1．37735-45．912μg（r=0．9996），最低检测限依次为0．21，0．07，0．22，0．22，0．27，0．23，0．24，0．24μg；6种中药提取物回收率测定结果满意。结论本方法简便、灵敏、准确，适用于不同中药提取物中大孔吸附树脂有机残留物的测定。OBJECTIVE To establish a method for the determination of 8 residua of n-hexane, benzene, toluene,o-Dimethyl benzene, p-dimethy benzene, phenylethene, diviylbe znene and 1,2-diethyl styrene from macroporous resin, in 6 kinds of Chinese medicine extract. METHODS The headspace GC system consisted of a capillary column , polymerization or cross linking polyethylene glycol as the solid phase, and FID as the detector. Column temperature was maintained at 60 ℃ for 16 minutes, then increased to 200 ℃ at 16 ℃ per minute, and at 200℃ for 2 minutes. RESULTS All of 8 residua were seperated and good linear responses were obtained in the following range, n - hexane1.386-46.2μg （r=0.997 5）, benzene 0.4749-15.83 μg （r=0.999 6）, toluene 1.488-49.6μg （r=0.999 3）, o-dimethyl benzene 1.4778-49.26 μg （r=0.999 1）, p-dimethy benzene 1.8183-60.61 μg （r=0.999 0）, phenylethene 1.547 4-51.58μg（r=0.999 5）, 1, 2-diethyl styrene 1.620 6-54.02 μg（r=0.998 1）, divinyl-benzene 1.377 35-45.912 μg （r=0.999 6）. The LOD were 0.21, 0.07, 0.22, 0.22, 0.27, 0.23, 0.24 and 0.24 μg, respectively. CONCLUSION The method is simple, convenient, sensitive and accurate, and it can be used to determine residuum from macroporous resin in Chinese medicine extracts, respectively.

关 键 词：中药提取物 大孔吸附树脂有机残留物 顶空进样 气相色谱法 

分 类 号：R917[医药卫生—药物分析学]