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-ECD和GC-NCI-MS测定方法。方法:采用固定相萃取净化杂质,DB-1701MS和HP-5MS弹性石英毛细管柱分离待测组分,ECD和NCI-MS分别检测。进样口温度:230℃,载气:N2(99.99%,ECD)和He2(99.999%,MS),柱流量:1.0 mi/min,不分流进样,进样量:1μL;ECD温度300℃;MS选择化学电离负离子源,离子源温度:200℃,电离能量:100 eV,传输管温度:290℃,反应气为甲烷,流量:3.0 mL/min,以全扫描方式(scan)定性,选择离子(SIM)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-1701柱上,甲基五氯苯硫醚和艾试剂重叠(ECD),氧氯丹和δ-666重叠(MS),而在HP-5柱上,环氧七氯和氧氯丹重叠,重叠的二成分采用ECD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δ-666中255m/z),采用选择离子方式(SIM)而同时分别定量。此外,除六氯苯、反氯丹、pp’-DDE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ECD低,定量限普遍比ECD高。结论:GC-ECD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-MS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-MS法具有快速、准确性强的优势,而GC-ECD法则具有灵敏度高、精密度好的优势。
AIM:To investigate the differences between GC-ECD and GC-MS methods which were employed in the determination of 20 organochlorine pesticide residues in Gancaoxin Granule(Radix et Rhizoma glycyrrhizae,zine preparation)and Fuxin Tablet(Folium Crataegi).METHODS:The solid-phase extraction was used for the clean-up of samples,the quartz capillary columns of DB-1701MS and HP-SMS were selected for the separations of target pesticides,ECD and MS were introduced as the detections respectively.N2(99.99%,ECD)and He2(99.999%,MS)were used as carries,a column flow was at 1.0 mL/min,splitless was chosen as injection mode,injection amount was 1 uL for all instances,the inlet was set at 230℃and ECD at 300℃,negative ions-chemical ionization was used as ion source in MS,the source temperature was set at 200℃,the electron energy was at 100 eV,and the temperature of transfer line was at 290%;methane was used as reagent gas with a flow of 3.0 mL/min,scan mode was for qualification,SIM mode was for quantitation.RESULTS:Because 20 organochlorine pesticides were impossible to be separated all on single column by an optimal temperature program to present maximum 19 peaks,on HP and column,both heptachlor-epoxide and oxy-chlordane appeared as a peak,while the overlaid peak in DB-1701 column was contributed by eicher pentachlorothioanisole and aldrin in ECD or oxy-chlordane andδ-666 in MS.We selected SIM mode in MS detection with different m/z and abundance to quantify.By a comparison,the residues of 20 organochlorine pesticides in two preparations showed higher in ECD than that in MS,except for hexachlorobenxene,trans-chlordane,pp'-DDE and endrin,the LOQs of 20 insecticides in ECD was commonly lower than that in MS.CONCLUSION:The ECD method has an advantage in sensitivity and precision,but its result on either qualification and quantitation is prone to the interferences of false positive peaks and background;while MS detection has high specificity in qualification and good accuracy in quantitation,but lower sensitivity and precision compared to ECD.Therefore,GC-ECD method for 20 organochlorine pesticide residues is sensitive and of good precision,while GC-MS method is rapid and accurate.
作者
郭青
邓鸣
宁青
余伯阳
GUO Qing;DEN Ming;NING Qing;YU Bo-yang(J.China Pharmaceutical University,Nanjing 210009,China;Jiangsu lnstituefor Drug Control,Na ng 210008,China;Nanjing University of Traditional Chinese Medicine,Nanjing 210046,China)
出处
《中成药》
CAS
CSCD
北大核心
2008年第11期1624-1628,共5页
Chinese Traditional Patent Medicine
