高效液相色谱-串联质谱法测定水稻中多杀霉素的残留及消解动态  

Study on decline and residue of spinosad in paddy using high performance liquid chromatography-tandem mass spectrometry

作　　者：李文明[1] 乔成奎[1] 陈晓旭[1] 李青阳[2] 李明慧[3] 李文希[3] 韩丽君[3] 

机构地区：[1]河南农业大学植物保护学院,郑州450002 [2]河南农业大学生命科学学院,郑州450002 [3]中国农业大学理学院,北京100193

出　　处：《农药学学报》2012年第3期298-304,共7页Chinese Journal of Pesticide Science

基　　金：河南省重大公益科研项目(102102110038)

摘　　要：采用高效液相色谱-串联质谱(HPLC-MS/MS)建立了水稻中多杀霉素的残留分析方法。样品经乙腈提取,乙二氨基-N-丙基硅烷(PSA)和石墨化碳黑(GCB)净化,HPLC-MS/MS检测。结果表明:多杀霉素A在0.006～1.2 mg/L范围内线性关系良好,相关系数(R2)为0.990 5;多杀霉素D在0.001～0.2 mg/L范围内线性关系良好,R2为0.994 9。多杀霉素A和D的检出限(LOD)在田水中均为0.001 mg/L,在稻田土壤、水稻植株、糙米、稻壳和稻杆中均为0.005 mg/kg;多杀霉素A和D的定量限(LOQ)在田水中均为0.005 mg/L,在稻田土及各水稻基质中分别为0.06和0.01 mg/kg。在添加水平为0.005～6.0 mg/kg范围内,稻田土壤、田水及水稻各基质中多杀霉素A和D的平均回收率为72.9%～107.9%,相对标准偏差(RSD)为1.7%～13.5%。采用该方法对多杀霉素在田间水稻中的消解动态和最终残留进行了测定。结果表明,多杀霉素在稻田土壤、田水和水稻植株样品中的消解均符合一级动力学方程,半衰期分别约为7.5、1.2和4.8 d,属于易降解农药。A residue analytical method of spinosad in paddy was established using high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） detection.The samples were extracted with acetonitrile,and purified on primary secondary amine（PSA） and graphitized carbon black（GCB）,finally analyzed by HPLC-MS/MS.The method showed good linearity in the ranges of 0.006-1.2 mg/L,0.001-0.2 mg/L for spinosyns A and D with correlation coefficients（R2） of 0.990 5 and 0.994 9 respectively.The limits of detection（LOD） for spinosyns A and D were 0.001 mg/L in paddy water,and 0.005 mg/kg in paddy soil,rice plants,rice,rice husk and rice straw.The limits of quantification（LOQ） for spinosyns A and D in paddy water were 0.005 mg/L,and with 0.06 mg/kg,0.01 mg/kg respectively in rice matrices.The average recoveries of spinosyn A and D in paddy soil,water and other rice samples at 0.005-6.0 mg/kg spiked level were 72.9%-107.9% with relative standard deviations（RSD） of 1.1%-13.5%.The decline study of spinosad residue in paddy soil,water and rice plants suggested that the decline curves accorded with the first-order kinetics equation,and the half-lives of spinosad were 7.5,1.2,4.8 d,respectively.Spinosad belongs to the easily degradable pesticides.

关 键 词：高效液相色谱-串联质谱 多杀霉素 水稻 残留 消解 

分 类 号：O657.63[理学—分析化学]