摘要
建立了同时检测大孔吸附树脂中苯、甲苯、二甲苯、苯乙烯、二乙苯、二乙烯苯、萘、癸烷、十一烷和十二烷等10种有机残留物的测定方法.以二氯甲烷为提取溶剂,采用超声提取法对样品进行前处理.采用气相色谱法检测,色谱柱为DB-624毛细管柱,检测器为氢火焰离子化检测器.上述10种有机残留物在12 min内能很好地分离,样品的加标回收率(n=3)为73.8%～107.9%,相对标准偏差为1.3%～4.4%,最低检测限为0.007～0.03 mg/L.本方法具有灵敏、准确、快速等特点.对9种商品树脂及其预处理品的有机残留物进行了测定,结果表明树脂预处理前后有机残留物的含量相差很大,经过预处理的树脂可以安全地应用于中药的生产.
A method has been developed for the simultaneous determination of benzene, toluene, xylene, styrene, decane, diethylbenzene, undecane, divinylbenzene, dodecane and naphthalene residues in macroporous adsorption resins （MARs）. The organic residues were extracted from resin samples by ultrasonic extraction with dichloromethane and analyzed by gas chromatography. The chromatographic conditions were as follows： a DB-624 capillary column （30m×0. 32 mm i. d., 1.8μm） ; carrier gas, nitrogen with a flow rate of 2.5 mL/min; column temperature, programmed from 40℃ to 200℃ at a rate of 14℃/min and kept at 200℃ for 1 min; flame ionization detector temperature, 250℃; injector temperature, 220℃; splitless injection, 1μL. All the 10 organic residues were separated well in 12 min. The recoveries for spiked standards （n=3） were 73.8%-107.9%. The relative standard deviations were 1.3%-4.4%. The limits of detection were 0.007-0.03mg/L. This method is sensitive, accurate and quick. Nine commercial MARs and their pretreated samples were assayed, and the results show that the contents of organic residues varied greatly in two kinds of samples. And the pretreated MARs can be used safely in the oroduction of traditional Chinese medicines.
出处
《色谱》
CAS
CSCD
北大核心
2005年第6期655-658,共4页
Chinese Journal of Chromatography
基金
"十五"国家科技攻关项目(2001BA701A02)
关键词
气相色谱法
苯
甲苯
二乙苯
萘
癸烷
有机残留物
大孔吸附树脂
gas chromatography
benzene
toluene
diethylbenzene
naphthalene
decane
organic residues
macroporous adsorption resin
作者简介
贾存勤，男，博士研究生，Tel：（010）82801404，E-mail：jiacunqin@tom．com
通讯联系人：屠鹏飞，男，教授，博士，博士生导师，Tel：（010）82802750，E-mail：pengfeitu@bjmu.edu.cn.
