采用GC_ECD和GC_MS分别测定并比较甘草锌颗粒及复心片中二十种有机氯农药残
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[质 量]采用GC 2ECD 和GC 2M S 分别测定并比较甘草锌颗粒及复心片中二十种有机氯农药残留量郭 青1,2, 邓 鸣1, 宁 青3, 余伯阳13(1.中国药科大学,江苏南京210009;2.江苏省药品检验所,江苏南京210008;3.南京中医药大学,江苏南京210046)收稿日期:2008203231作者简介:郭 青(1964-),女,主任药师,在职博士生,研究方向:中药分析与质量标准,电话:025*********,E 2mail:guoqing850@yahoo .cn 。
3通讯作者:余伯阳,电话:025*********,E 2mail:boyangyu@yahoo ,boyangyu59@ 。
关键词:20种有机氯农药(OCPs );GC 2ECD (电子捕获检测);GC 2MS;负化学离子源(N I C I );选择离子监测(SI M );甘草锌颗粒;复心片摘要:目的:探索并比较2种中成药中20种有机氯农药残留量的GC 2ECD 和GC 2NC I 2M S 测定方法。
方法:采用固定相萃取净化杂质,DB 21701MS 和HP 25M S 弹性石英毛细管柱分离待测组分,ECD 和NC I 2M S 分别检测。
进样口温度:230℃,载气:N 2(99.99%,ECD )和He 2(99.999%,MS ),柱流量:1.0m i/m in,不分流进样,进样量:1μL;EC D 温度300℃;MS 选择化学电离负离子源,离子源温度:200℃,电离能量:100e V,传输管温度:290℃,反应气为甲烷,流量:3.0mL /m in,以全扫描方式(scan )定性,选择离子(SI M )方式定量。
结果:20种有机氯在2根毛细管柱上不可能通过调整升温程序来达到全部分离,最多可检测到19个峰,在DB 21701柱上,甲基五氯苯硫醚和艾试剂重叠(ECD ),氧氯丹和δ2666重叠(M S ),而在HP 25柱上,环氧七氯和氧氯丹重叠,重叠的二成分采用EC D 检测无法定量;而用MS 检测则可通过寻找一定丰度的不同质荷比特征离子(如氧氯丹中316m /z 和δ2666中255m /z ),采用选择离子方式(SI M )而同时分别定量。
此外,除六氯苯、反氯丹、pp ’2DDE 和异狄试剂外,二种制剂中的20种有机氯残留的MS 数据普遍比EC D 低,定量限普遍比EC D 高。
结论:GC 2EC D 法对于痕量级的农药残留检测具有灵敏度高和精密度好的优势,但定性和定量均易受假阳性及背景的干扰;而GC 2MS 法定性专属,定量也不受干扰,但检测灵敏度和精密度均不及ECD 。
因此,对于本试验中20种有机氯的测定,GC 2M S 法具有快速、准确性强的优势,而GC 2EC D 法则具有灵敏度高、精密度好的优势。
中图分类号:R927.1 文献标识码:A 文章编号:100121528(2008)1121624205D eter m i n a ti on of 20organochlor i n e pesti c i de resi dues i n Gancaox i n Granule and Fux i n Tablet by GC 2ECD and GC 2M S respecti vely and co m par ison s between the two m ethodsG UO Q ing 1,2, DE N M ing 1, N I N G Q ing 3, Y U Bo 2yang13(1.China Phar m aceutical U niversity,N anjing 210009,China; 2.J iangsu Institue for D rug Control,N anjing 210008,China; 3.N anjing U niversity ofTraditional Chinese M edicine,N anjing 210046,China )KE Y WO R D S :20organochl orine pesticide residues (OCPs );GC 2ECD (electr on cap ture detecti on );GC 2MS;negative i on che m ical i onizati on (N I C I );selected i ons monit oring (SI M );Gancaoxin Granule;Fuxin Tablet ABSTRACT:A I M :T o investigate the differences bet w een GC 2ECD and GC 2MS methods which were e mp l oyed in the deter m inati on of 20organochl orine pesticide residues in Gancaoxin Granule (R adix et R h izo m a glycyrrhizae,zine prepa ration )and Fuxin Tablet (Folium C rataeg i ).M ETHOD S :The s olid 2phase extracti on was used for theclean 2up of sa mp les,the quartz cap illary colu mns of DB 21701M S and HP 25M S were selected f or the separati ons of tar 2get pesticides,ECD and MS were intr oduced as the detecti ons res pectively .N 2(99.99%,ECD )and He 2(99.999%,MS )were used as carries,a column fl ow was at 1.0mL /m in,s p litless was chosen as injecti on mode,injecti on a mount was 1μL for all instances,the inlet was set at 230℃and ECD at 300℃,negative i ons 2che m ical4261i onizati on was used as i on s ource in MS,the s ource te mperature was set at200℃,the electr on energy was at100 e V,and the te mperature of transfer line was at290℃;methane was used as reagent gas with a fl ow of3.0mL/ m in,scan mode was f or qualificati on,SI M mode was for quantitati on.RESU L TS:Because20organochl orine pes2 ticides were i m possible t o be separated all on single colu mn by an op ti m al te mperature p r ogra m t o p resent maxi m um 19peaks,on HP and colu mn,both hep tachl or2epoxide and oxy2chl ordane appeared as a peak,while the overlaid peak in DB21701colu mn was contributed by eicher pentachl or othi oanis ole and aldrin in ECD or oxy2chl ordane and δ2666in MS.W e selected SI M mode in MS detecti on with different m/z and abundance t o quantify.By a compari2 s on,the residues of20organochl orine pesticides in t w o p reparati ons showed higher in ECD than that in MS,excep t for hexachl or obenxene,trans2chl ordane,pp’2DDE and endrin,the LOQ s of20insecticides in ECD was commonly l o wer than that in MS.CO NCL US I O N:The ECD method has an advantage in sensitivity and p recisi on,but its re2 sult on either qualificati on and quantitati on is p r one t o the interferences of false positive peaks and backgr ound; while MS detecti on has high s pecificity in qualificati on and good accuracy in quantitati on,but l ower sensitivity and p recisi on co mpared t o ECD.Theref ore,GC2ECD method for20organochl orine pesticide residues is sensitive and of good p recisi on,while GC2MS method is rap id and accurate. 中药材和中成药的安全性已成为世界关注的问题,世界发达国家和地区对植物药和植物提取物中的农药残留量都有严格的规定和限制,中药欲与国际接轨,按照国际或进口国家及使用地区标准检测农药残留量则十分必要和迫切[123]。
20种有机氯农药残留是香港卫生署规定的内地中药在香港上市的必检项目[3],根据异构体和降解产物被分成7大类,最大残留限量是按照各类中的农药原体、异构体和降解产物之和而制定的。
