顶空气相色谱测定灯盏花素提取物中大孔树脂有机溶剂残留物  

Determination of macro-porous resin residua in Breviscapin extract by headspace gas chromatography

作　　者：许勇[1] 郏征伟[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：《中成药》2011年第8期1351-1355,共5页Chinese Traditional Patent Medicine

摘　　要：目的建立灯盏花素提取物中8种大孔树脂有机溶剂残留物的检测方法。方法采用顶空进样毛细管气相色谱法,色谱柱为HP-INNOWAX毛细管柱(30 m×0.53 mm×1.0μm),柱温起始温度60℃,维持16 min,再以每分钟20℃升温至200℃,维持2 min;进样口温度240℃;FID检测器温度300℃。结果在此条件下,待测物正己烷、苯、甲苯、对二甲苯、邻二甲苯、苯乙烯、12,-二乙基苯、二乙烯苯与内标物正丁醇获得了较好的分离。8种成分在各自的质量浓度范围内呈良好的线性关系(r=0.999,n=7),平均回收率为82.51%～94.92%,RSD为4.9%～6.5%,最低检出限范围为0.02～0.57μg/g。结论该方法简便快速、结果准确、重现性好,可用于灯盏花素提取物中大孔树脂有机溶剂残留量的测定。AIM To establish a method for detecting the residues of macro-prous resin in the extract of Breviscapin.METHODS Headspace GC was used with INNOWAX column（30 m×0.53 mm ×1.0 μm）.Column temperature was maintained at 60 ℃ for 16 minutes,then increased to 200 ℃ at 16 ℃ per minute for 2 minutes.The injector temperature was 240 ℃ and FID detector temperature was 300 ℃.RESULTS Under the qualitative conditions,all of the eight residues,including n-hexane,benzene,methybenzene p-xylene,o-xylene,phenylethylene,1,2-diethylenzene,and o-divinylbenzene,were separated and good linear responses were obtained in the experimental concentration（r=0.999,n=7）.The average recoveries of the eight residues were in the range of 82.51%-94.92%,with RSD of 4.9%-6.5%.The LODs were 0.02-0.57μg/g.CONCLUSION The analytical method is proved to be convenient and accurate which can be used to determine macro-prous residues in the extract of Breviscapin.

关 键 词：大孔树脂有机残留物 顶空进样 气相色谱法 灯盏花素提取物 

分 类 号：R297[医药卫生—民族医学]