快速溶剂萃取-气相色谱-串联质谱法同时测定土壤中有机氯及有机磷农药
|
摘要
建立了快速溶剂萃取(ASE)-气相色谱-串联质谱(GC-MS/MS)同时分析土壤中8种有机氯农药(OCPs)和5种有机磷农药(OPPs)的方法。样品由正己烷-丙酮(1∶1,v/v)溶液萃取,经无水硫酸钠脱水、氮吹仪浓缩后,采用硅胶(Si)固相萃取小柱进行净化,正己烷-丙酮(1∶1,v/v)溶液进行洗脱,然后经HP-5MS色谱柱(30 m×0. 25 mm×0. 25μm)分离,在电子轰击电离源下以多反应监测(MRM)模式进行检测,内标法定量。分析结果表明,13种目标物在1. 00~100μg/L范围内线性关系良好,相关系数(R)大于0. 995;加标回收率为66. 8%~88. 4%,能够实现准确定量;日内精密度与日间精密度均小于10%。当取样量为10. 0 g时,8种OCPs的方法检出限为0. 02~0. 04μg/kg,5种OPPs的方法检出限为0. 06~0. 12μg/kg,能够满足土壤农药残留的检测要求。
A method based on gas chromatography-tandem mass spectrometry(GC-MS/MS)coupled with accelerated solvent extraction(ASE)was developed for the determination of eight organochlorine pesticides(OCPs)and five organophosphorus pesticides(OPPs)in soils. The soil samples were grinded after freeze-drying. Particles with diameters lower than 250 μm were chosen by ion-sieving. After this,10. 0 g soil mixed with 2. 0 g diaomite was extracted with hexane-acetone(1 ∶1,v/v). The extracts were dehydrated with anhydrous sodium sulfate and concentrated with a termovap sample concentrator. The concentrated solutions were further cleaned up with Si SPE columns and eluted with hexane-acetone(1 ∶1,v/v). The purified solutions were then isolated by HP-5 MS column(30 m×0. 25 mm×0. 25 μm)and detected using the multiple reaction monitoring mode at the electron impact source. It is observed that this method has good linearities in the range of 1. 00-100 μg/L for the 13 compounds,and the correlation coefficients(R)were greater than 0. 995. The spiked recoveries of the 13 compounds were in the range of 66. 8%-88. 4%,and the relative standard deviations were less than 10%. With 10. 0 g of sampling weight,the method detection limits ranged from 0. 02 to 0. 04 μg/kg for the eightOCPs and from 0. 06 to 0. 12 μg/kg for the five OPPs. This method is suitable for the determination of trace OCPs and OPPs in soils.
A method based on gas chromatography-tandem mass spectrometry(GC-MS/MS)coupled with accelerated solvent extraction(ASE)was developed for the determination of eight organochlorine pesticides(OCPs)and five organophosphorus pesticides(OPPs)in soils. The soil samples were grinded after freeze-drying. Particles with diameters lower than 250 μm were chosen by ion-sieving. After this,10. 0 g soil mixed with 2. 0 g diaomite was extracted with hexane-acetone(1 ∶1,v/v). The extracts were dehydrated with anhydrous sodium sulfate and concentrated with a termovap sample concentrator. The concentrated solutions were further cleaned up with Si SPE columns and eluted with hexane-acetone(1 ∶1,v/v). The purified solutions were then isolated by HP-5 MS column(30 m×0. 25 mm×0. 25 μm)and detected using the multiple reaction monitoring mode at the electron impact source. It is observed that this method has good linearities in the range of 1. 00-100 μg/L for the 13 compounds,and the correlation coefficients(R)were greater than 0. 995. The spiked recoveries of the 13 compounds were in the range of 66. 8%-88. 4%,and the relative standard deviations were less than 10%. With 10. 0 g of sampling weight,the method detection limits ranged from 0. 02 to 0. 04 μg/kg for the eightOCPs and from 0. 06 to 0. 12 μg/kg for the five OPPs. This method is suitable for the determination of trace OCPs and OPPs in soils.
引文
[1] Fu J M,Mai B X,Sheng G Y,et al. Chemosphere,2003,52(9):1411
[2] Zhang X T,Lu Y S,Yang D. China Environmental Science,2016,36(7):2146张晓涛,陆愈实,杨丹.中国环境科学,2016,36(7):2146
[3] Sun X J,Guo M M,Wang S Y,et al. Chinese Journal of Chromatography,2014,32(10):1124孙晓杰,郭萌萌,王苏玥,等.色谱,2014,32(10):1124
[4] Cao Z Y,Mu R X,Wu L,et al Chinese Journal of Chromatography,2014,32(12):1390曹赵云,牟仁祥,吴俐,等.色谱,2014,32(12):1390
[5] Ren K Y,Zhang W L,Cao S R. Chinese Journal of Analytical Chemistry,2017,45(11):1669任科宇,张文林,曹淑瑞.分析化学,2017,45(11):1669
[6] HJ 911-2017
[7] Si X X,Zhu R Z,Zhang F M,et al. Chinese Journal of Chromatography,2016,34(6):608司晓喜,朱瑞芝,张凤梅,等.色谱,2016,34(6):608
[8] HJ 783-2016
[9] Zhang R J,Yao Y X,Dang J H,et al. Safety and Environmental Engineering,2017,24(4):74张瑞娟,姚宇霞,党晋华,等.安全与环境工程,2017,24(4):74
[10] Huang Z,Fan L. Technology&Development of Chemical Industry,2014,43(11):46黄志,范磊.化工技术与开发,2014,43(11):46
[11] Li Z Y,Zhou X Y. Environment and Development,2017(4):159李钟瑜,周晓颖.环境与发展,2017(4):159
[12] Liu X,Kong W H,Shang S J,et al. Analytical Instrumentation,2017(4):147刘鑫,孔维恒,尚士进,等.分析仪器,2017(4):147
[13] EPA method 3545
[14] HJ 921-2017
[15] Guo H H,Chen G,Ma J T,et al. Chinese Journal of Chromatography,2017,35(3):328郭会华,陈刚,马久彤,等.色谱,2017,35(3):328
[16] Peng X J,Qin H,Wen Q J,et al. Chinese Journal of Chromatography,2016,34(8):817彭晓俊,秦汉,温绮靖,等.色谱,2016,34(8):817
[17] HJ 768-2015
[18] HJ 835-2017
[19] Du J,LüB,Zhu P,et al. Chinese Journal of Chromatography,2013,31(8):739杜娟,吕冰,朱盼,等.色谱,2013,31(8):739
[20] Zhu H Y,Liu W Y,Ding X N,et al. Chinese Journal of Chromatography,2011,29(8):773朱恒怡,柳文媛,丁曦宁,等.色谱,2011,29(8):773
[21] Liu J,Ding T,Yin D L,et al. Environmental Chemistry,2016,35(1):222刘晶,丁涛,尹丹莉,等.环境化学,2016,35(1):222
[2] Zhang X T,Lu Y S,Yang D. China Environmental Science,2016,36(7):2146张晓涛,陆愈实,杨丹.中国环境科学,2016,36(7):2146
[3] Sun X J,Guo M M,Wang S Y,et al. Chinese Journal of Chromatography,2014,32(10):1124孙晓杰,郭萌萌,王苏玥,等.色谱,2014,32(10):1124
[4] Cao Z Y,Mu R X,Wu L,et al Chinese Journal of Chromatography,2014,32(12):1390曹赵云,牟仁祥,吴俐,等.色谱,2014,32(12):1390
[5] Ren K Y,Zhang W L,Cao S R. Chinese Journal of Analytical Chemistry,2017,45(11):1669任科宇,张文林,曹淑瑞.分析化学,2017,45(11):1669
[6] HJ 911-2017
[7] Si X X,Zhu R Z,Zhang F M,et al. Chinese Journal of Chromatography,2016,34(6):608司晓喜,朱瑞芝,张凤梅,等.色谱,2016,34(6):608
[8] HJ 783-2016
[9] Zhang R J,Yao Y X,Dang J H,et al. Safety and Environmental Engineering,2017,24(4):74张瑞娟,姚宇霞,党晋华,等.安全与环境工程,2017,24(4):74
[10] Huang Z,Fan L. Technology&Development of Chemical Industry,2014,43(11):46黄志,范磊.化工技术与开发,2014,43(11):46
[11] Li Z Y,Zhou X Y. Environment and Development,2017(4):159李钟瑜,周晓颖.环境与发展,2017(4):159
[12] Liu X,Kong W H,Shang S J,et al. Analytical Instrumentation,2017(4):147刘鑫,孔维恒,尚士进,等.分析仪器,2017(4):147
[13] EPA method 3545
[14] HJ 921-2017
[15] Guo H H,Chen G,Ma J T,et al. Chinese Journal of Chromatography,2017,35(3):328郭会华,陈刚,马久彤,等.色谱,2017,35(3):328
[16] Peng X J,Qin H,Wen Q J,et al. Chinese Journal of Chromatography,2016,34(8):817彭晓俊,秦汉,温绮靖,等.色谱,2016,34(8):817
[17] HJ 768-2015
[18] HJ 835-2017
[19] Du J,LüB,Zhu P,et al. Chinese Journal of Chromatography,2013,31(8):739杜娟,吕冰,朱盼,等.色谱,2013,31(8):739
[20] Zhu H Y,Liu W Y,Ding X N,et al. Chinese Journal of Chromatography,2011,29(8):773朱恒怡,柳文媛,丁曦宁,等.色谱,2011,29(8):773
[21] Liu J,Ding T,Yin D L,et al. Environmental Chemistry,2016,35(1):222刘晶,丁涛,尹丹莉,等.环境化学,2016,35(1):222