工业安全与环保
工業安全與環保
공업안전여배보
INDUSTRIAL SAFETY AND ENVIRONMENTAL PROTECTION
2014年
12期
4-7
,共4页
吴海兵%曾鸿鹄%梁延鹏%莫凌云
吳海兵%曾鴻鵠%樑延鵬%莫凌雲
오해병%증홍곡%량연붕%막릉운
一体化固相萃取%GC-ECD%有机氯农药
一體化固相萃取%GC-ECD%有機氯農藥
일체화고상췌취%GC-ECD%유궤록농약
integrated solid phase extraction%GC-ECD%organochlorine pesticides
建立了采用一体化固相萃取提取和净化、GC-MS/GC-ECD联合定性定量同时检测水中14种有机氯农药的方法,优化了固相萃取和色谱条件。样品于一体化固相萃取仪上以10 mL/min流速经C18柱富集、6 mL体积比为1∶1的二氯甲烷/乙酸乙酯混合溶剂洗脱、氮吹浓缩后,GC-MS/GC-ECD分离检测。结果表明,14种OCPs在1.00~500μg/L范围内线性良好,方法检出限为1.76~15.10ng/L,平均加标回收率为69.6%~102.8%,RSD为1.62%~18.9%。实际样品分析表明该方法灵敏度和精密度高、准确性好、操作简便,适用于大批量水样中微量和痕量OCPs的测定。
建立瞭採用一體化固相萃取提取和淨化、GC-MS/GC-ECD聯閤定性定量同時檢測水中14種有機氯農藥的方法,優化瞭固相萃取和色譜條件。樣品于一體化固相萃取儀上以10 mL/min流速經C18柱富集、6 mL體積比為1∶1的二氯甲烷/乙痠乙酯混閤溶劑洗脫、氮吹濃縮後,GC-MS/GC-ECD分離檢測。結果錶明,14種OCPs在1.00~500μg/L範圍內線性良好,方法檢齣限為1.76~15.10ng/L,平均加標迴收率為69.6%~102.8%,RSD為1.62%~18.9%。實際樣品分析錶明該方法靈敏度和精密度高、準確性好、操作簡便,適用于大批量水樣中微量和痕量OCPs的測定。
건립료채용일체화고상췌취제취화정화、GC-MS/GC-ECD연합정성정량동시검측수중14충유궤록농약적방법,우화료고상췌취화색보조건。양품우일체화고상췌취의상이10 mL/min류속경C18주부집、6 mL체적비위1∶1적이록갑완/을산을지혼합용제세탈、담취농축후,GC-MS/GC-ECD분리검측。결과표명,14충OCPs재1.00~500μg/L범위내선성량호,방법검출한위1.76~15.10ng/L,평균가표회수솔위69.6%~102.8%,RSD위1.62%~18.9%。실제양품분석표명해방법령민도화정밀도고、준학성호、조작간편,괄용우대비량수양중미량화흔량OCPs적측정。
We developed an integrated method that combined solid -phase extraction and purification, GC -MS/GC -ECD for qualitative and quantitative determining 14 organochlorine pesticides in water. The solid -phase extraction and chromatography condition were optimized. The sample was extracted on the integrated method with 10 mL/min velocity by C18 column enrichment, eluted by 6 mL mixed solution of dichloromethane/ethyl acetate with the volume ratit of 1∶1 and concentrated by nitrogen, and was separated and detected by GC-MS/GC-ECD. The results indicate that 14 OCPs show a good linearity in the range of 1. 00~500μg/L. The detection limit was 1. 76~15. 10 ng/L, the average recovery was 69. 6% ~102. 8%, RSD was 1. 62% ~18. 9%. The analysis of actual samples demonstrate that this method shows high sensitivity and precision, good accuracy, simple operation, and suitable for determination of trace and ultra-trace OCPs in water samples.