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

 目的建立测定6种中药提取物中正己烷、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16 min,以每分钟20℃的升温速率升至200℃,保持2 min。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=0.997 5),苯0.474 9～15.83μg(r=0.999 6),甲苯1.488～49.6μg(r=0.999 3),对二甲苯1.477 8～49.26μg(r=0.999 1),邻二甲苯1.818 3～60.61μg(r=0.999 0),苯乙烯1.547 4～51.58μg(r=0.999 5),1,2-二乙基苯1.6206～54.02μg(r=0.998 1)和二乙烯苯1.377 35～45.912μg(r=0.999 6),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。

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

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-hexane1.386-46.2 μg(r=0.997 5),benzene 0.4749-15.83 μg(r=0.999 6),toluene 1.488-49.6 μg(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 4-51.58 μg(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.