中国中医药信息杂志
中國中醫藥信息雜誌
중국중의약신식잡지
CHINESE JOURNAL OF INFORMATION ON TRADITIONAL CHINESE MEDICINE
2014年
1期
74-78
,共5页
大枣%气相色谱法%有机氯农药%拟除虫菊酯农药
大棘%氣相色譜法%有機氯農藥%擬除蟲菊酯農藥
대조%기상색보법%유궤록농약%의제충국지농약
Zigyphussp%gas chromatography%organochlorine pesticides%pyrethroid pesticides
目的:建立快速同时测定大枣中50种有机氯及拟除虫菊酯农药残留的气相色谱测定方法。方法样品用加速溶剂萃取法(ASE)萃取,以乙腈(1%乙酸)为提取溶剂,温度100℃,静态萃取5 min,循环3次,提取液用Florisil 硅土柱净化,乙酸乙酯-正己烷(15∶85,V/V)洗脱,采用 HP-5与 DB1701毛细管色谱柱双柱定性,以HP-5毛细管柱定量,GC-ECD检测器进行检测。结果样品3水平添加时的50种有机氯及拟除虫菊酯农药平均回收率为71.4%~110.9%,RSD为1.2%~14.1%,符合农药残留分析的要求。结论本方法仪器简单,使用范围广,重复性及净化效果好,可用于大枣中50种有机氯及拟除虫菊酯类农药残留量检测。
目的:建立快速同時測定大棘中50種有機氯及擬除蟲菊酯農藥殘留的氣相色譜測定方法。方法樣品用加速溶劑萃取法(ASE)萃取,以乙腈(1%乙痠)為提取溶劑,溫度100℃,靜態萃取5 min,循環3次,提取液用Florisil 硅土柱淨化,乙痠乙酯-正己烷(15∶85,V/V)洗脫,採用 HP-5與 DB1701毛細管色譜柱雙柱定性,以HP-5毛細管柱定量,GC-ECD檢測器進行檢測。結果樣品3水平添加時的50種有機氯及擬除蟲菊酯農藥平均迴收率為71.4%~110.9%,RSD為1.2%~14.1%,符閤農藥殘留分析的要求。結論本方法儀器簡單,使用範圍廣,重複性及淨化效果好,可用于大棘中50種有機氯及擬除蟲菊酯類農藥殘留量檢測。
목적:건립쾌속동시측정대조중50충유궤록급의제충국지농약잔류적기상색보측정방법。방법양품용가속용제췌취법(ASE)췌취,이을정(1%을산)위제취용제,온도100℃,정태췌취5 min,순배3차,제취액용Florisil 규토주정화,을산을지-정기완(15∶85,V/V)세탈,채용 HP-5여 DB1701모세관색보주쌍주정성,이HP-5모세관주정량,GC-ECD검측기진행검측。결과양품3수평첨가시적50충유궤록급의제충국지농약평균회수솔위71.4%~110.9%,RSD위1.2%~14.1%,부합농약잔류분석적요구。결론본방법의기간단,사용범위엄,중복성급정화효과호,가용우대조중50충유궤록급의제충국지류농약잔류량검측。
Objective To establish a gas chromatography method for the determination of 50 organochlorine and pyrethroid pesticides residues in Zigyphussp. Methods The organochlorine and pyrethroid pesticides were extracted from Zigyphussp with solvents of acetonitrile (1%acetic acid) by accelerated solvent extraction (ASE) for 5 min at 100℃. Then the extracts were cleaned up by alumina neutral-florisil column and eluted by mixed solvents of ethyl acetate and hexane (15∶85, V/V). The extract was separated by HP-5 and DB1701 capillary dual-column and detected by electron-capture detector. Results The average recoveries and RSD ranged from 71.4% to 110.9%and 1.2% to 14.1% respectively, at three spiked mixed organochlorine and pyrethroid levels. Conclusion The method has good separation and repeatability, and can be used in determination of organochlorine and pyrethroid pesticide residues in Zigyphussp.