水中13种有机磷农药的固相萃取-气相色谱-质谱测定法  

Determination of 13 Kinds of Organic Phosphorus Pesticides in Water Using Gas Chromatography-Mass Spectrometer with Solid-Phase Extraction

作　　者：高玲[1] 杨元[1] 景露[1] 谯斌宗 

机构地区：[1]成都市疾病预防控制中心理化检验科,四川成都610041 [2]成都市食品药品检验中心,四川成都610041

出　　处：《环境与健康杂志》2009年第8期723-725,共3页Journal of Environment and Health

摘　　要：目的建立水中13种有机磷农药的固相萃取-气相色谱-质谱测定方法。方法采用石墨化碳-氨基复合型柱对水样进行固相萃取(SPE)后,使用DB-1701P型弹性石英毛细管柱分离,以气相色谱-质谱法测定水中13种有机磷农药(敌敌畏、速灭磷、甲拌磷、二嗪磷、赛福丁已胺磷、乐果、甲基对硫磷、马拉硫磷、杀螟硫磷、对硫磷、稻丰散、杀扑磷、乙硫磷)。以二氯甲烷为洗脱溶剂,进样口温度为280℃,柱流量为1.2ml/min。结果在0.05～2.5mg/L线性范围内,敌敌畏的检出限为0.49μg/L;在0.10～2.5mg/L线性范围内,速灭磷的检出限为1.4μg/L;在0.05～2.5mg/L线性范围内,甲拌磷的检出限为0.96μg/L;在0.05～2.5mg/L线性范围内,二嗪磷的检出限为0.73μg/L;在0.05～2.5mg/L线性范围内,赛福丁已胺磷的检出限为0.60μg/L;在0.05～2.5mg/L线性范围内,乐果的检出限为1.8μg/L;在0.10～2.5mg/L线性范围内,甲基对硫磷的检出限为2.2μg/L;在0.05～2.5mg/L线性范围内,马拉硫磷的检出限为0.34μg/L;在0.05～2.5mg/L线性范围内,杀螟硫磷的检出限为1.1μg/L;在0.10～2.5mg/L线性范围内,对硫磷的检出限为0.58μg/L;在0.05～2.5mg/L线性范围内,稻丰散的检出限为1.2μg/L;在0.05～2.5mg/L线性范围内,杀扑磷的检出限为0.77μg/L;在0.50～2.5mg/L线性范围内,乙硫磷的检出限为0.26μg/L,相关系数均≥0.99。该方法所得的平均回收率为94.40%～100.80%,RSD为4.17%～14.73%。结论该方法具有操作简便、快速,灵敏度高,结果准确的优点,适用于环境水样中13种有机磷农药的同时测定。Objective To develop a method for the determination of 13 kinds of organic phosphorus pesticides in the water by gas chromatography-mass spectrometry with solid phase extraction （SPE）. Methods The 13 organic phosphorus pesticide residues, including dichlorvos, mevinphos, phorate, diazinon, propetamphos, ddimethoate, methyl parathion, malathion, fenitrothion, parathion, phenthion, methidathion, ethion, were separated on DB-1701P elastic silica capillary column followed by SPE with carbon-amino group complicated column and analyzed by gas chromatography mass spectrometry. Methylene dichloride was elution solvent,injection inlet temperature was 280℃ and column flow rate was 1.2 ml/min. Results The leaner range and limit of detection was 0.05-2.5 mg/L,0.49ug/L for dichlorvos;0.10-2.5 mg/L,1.4ug/L for mevinphos;0.05-2.5 mg/L,0.96 ug/L for phorate;0.05-2.5 mg/L,0.73 ug/L for diazinon;0.05-2.5 mg/L,0.60 ug/L for propetamphos;0.05-2.5 mg/L,1.8ug/L for ddimcthoate;0.10-2.5 mg/L,2.2ug/L for methyl parathion;O.05-2.5 rag/L,0.34 ug/L for malathion;0.05-2.5 mg/L, 1.1 ug/L for fenitrothion;0.10-2.5 mg/L,0.58 ug/L for parathion;0.05-2.5 rag/L,1.2 ug/L for phenthion;0.05-2.5 rag/L,0.77 ug/L for methidathion;0.50-2.5 mg/L, 0.26 ug/L for ethion. For all thirteen organic phosphorus pesticides, the correlation coefficient was above 0.99. The average recovery rates were 94.40%-100.80% and RSDs were found in the range of 4.17%-14.73%. Conclusion The method is simple,rapid,sensitive, accurate and applicable to the simultaneous determination of 13 kinds of organic phosphorus pesticide residues in water.

关 键 词：水 有机磷农药 固相萃取 色谱法 气相 质谱 

分 类 号：O657.6[理学—分析化学]