超声波提取-硫酸净化-气相色谱/质谱法同时测定土壤样品中23种有机氯农药
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摘要
建立了测定土壤样品中23种有机氯农药(OCPs)的GC-MS法。通过优化前处理条件,选择丙酮+石油醚作为提取剂,超声波提取30 min,上清液经氮吹浓缩,浓H2SO4净化,用GC-M S对化合物进行测定。结果表明,各化合物相关系数r≥0. 997。23种OCPs的方法精密度<9. 0%;加标回收率为56. 2%～107. 3%;检测限为0. 10～4. 0μg/kg。方法适用于大批量土壤样品中23种OCPs的快速测定。
A method was established for simultaneous determination of twenty-three organochlorine pesticides( OCPs) in soil using gas chromatography/mass spectrometry( GC-MS). Through the optimization of pre-treatment conditions,we chose acetone-petroleum ether as extracting agent. By ultrasonic extraction for 30 min,supernatant fluid was enrichment by nitrogen blow and purified by sulphuric acid. All these compounds were determined by GC-MS. The experimental results show that the calibration curves have good liner relationship( r ≥0. 997). The recoveries and limit of dection were 56. 2% ～ 107. 3% and 0. 10 ～ 4. 0 μg/kg with the relative standard deviations( RSD) less than9. 0% for 23 OCPs. The method could be applied analyze 23 OCPs in bulk soil samples.
A method was established for simultaneous determination of twenty-three organochlorine pesticides( OCPs) in soil using gas chromatography/mass spectrometry( GC-MS). Through the optimization of pre-treatment conditions,we chose acetone-petroleum ether as extracting agent. By ultrasonic extraction for 30 min,supernatant fluid was enrichment by nitrogen blow and purified by sulphuric acid. All these compounds were determined by GC-MS. The experimental results show that the calibration curves have good liner relationship( r ≥0. 997). The recoveries and limit of dection were 56. 2% ～ 107. 3% and 0. 10 ～ 4. 0 μg/kg with the relative standard deviations( RSD) less than9. 0% for 23 OCPs. The method could be applied analyze 23 OCPs in bulk soil samples.
引文
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[3] Ling B H,Ren Z Y,Chen H H,et al. J. Agro. Environ. Sci.,2007,26(5):1714李炳华,任仲宇,陈鸿汉,等.农业环境科学学报,2007,26(5):1714
[4] Qiu Y W,Zhang G,Guo L L,et al. Acta Oceanol. Sin.,2007,29(2):51丘耀文,张干,郭玲利,等.海洋学报,2007,29(2):51
[5] Li X M,Zhang Q H,Gan Y P,et al. Chin. J. Appl. Environ. Biol.,2007,13(6):901李雪梅,张庆华,甘一萍,等.应用与环境生物学报,2007,13(6):901
[6] Feng Y P,Liu H P,Ju P,et al. Chin. J. Anal. Lab.,2014,33(8):924封跃鹏,刘海萍,鞠平,等.分析试验室,2014,33(8):924
[7] Sun J H,Wang G L,Zhang G,et al. Environ. Sci.,2007,28(6):1332孙剑辉,王国良,张干,等.环境科学,2007,28(6):1332
[8] Nan S Q,Zhou P J,Rong Z,et al. Environ. Monit. Chin.,2009,25(6):81南淑清,周培疆,戎征,等.中国环境监测,2009,25(6):81
[9] Jiang Y F,Wang X T,Sun Y Z,et al. Environ. Sci.,2010,31(2):409蒋煜峰,王学彤,孙阳昭,等.环境科学,2010,31(2):409
[10] Jin G Y,Wang T Y,Yan L,et al. Environ. Sci.,2010,31(5):1359金光远,王铁宇,颜丽,等.环境科学,2010,31(5):1359
[11] Ma J S,Wang X,Wang H J,et al. Phys. Testing Chem. Anal. B,2014,50(6):740马健生,王鑫,王海娇,等.理化检验:化学分册,2014,50(6):740
[12] Tong L,Huang Y Y,Zhang L J,et al. Phys. Testing Chem. Anal. B,2009,45(7):858佟玲,黄园英,张玲金,等.理化检验:化学分册,2009,45(7):858
[13] Feng D,Yan Z,Zhang Y K,et al. Chin. J. Anal. Lab.,2005,24(10):8封棣,阎正,赵亚奎,等.分析试验室,2005,24(10):8
[14] GB/T 14550-2003,Method of gas chromatographic for determination of BHC and DDT in soil.GB/T 14550-2003,土壤中六六六和滴滴涕的测定.
[15] NY/T 761-2008,Pesticide multiresidue screen methods for determination of organophosphorus pesticides,organochlorine pesticides,pyrethroid pesticides and carbamate pesticedes in vegetables and fruits.NY/T 761-2008,蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定.