植物源性食品中46种农药多残留的分析方法
植物源性食品中46种农药多残留的分析方法? 样品前处理方法? 仪器分析方法仪器:岛津GCMS-TQ 8030气质联用仪载气:氦气色谱柱:Rtx-5MS,30 m×0.25 mm×0.25 μm载气流速:1 mL/min柱温: 碰撞气:氩气 进样口温度:250oC进样方式:不分流进样(1 min)接口温度:250oC进样量:1 μL离子源温度:250oC检测模式:多反应监测(MRM) ? 结果将空白样品(苹果、茄子、绿茶、大米)添加0.05 mg/kg的46种农药后,按上述前处理及仪器分析方法,使用对应的维泰克QuEChERS试剂包,采用基质匹配的校准曲线,平行三份样品考察添加回收率和相对标准偏差(RSD),结果如下表所示,46种农药的加标回收率在72.5-120.6%之间,相对标准偏差小于14.2%。编号农药苹果茄子绿茶大米回收率 (%)RSD(%)回收率 (%)RSD(%)回收率(%)RSD(%)回收率(%)RSD(%)1敌敌畏78.28.780.39.276.56.274.38.22甲拌磷95.66.3102.54.282.36.892.58.53alpha-六六六105.36.585.22.192.59.282.83.24乐果102.58.280.810.297.58.983.712.15beta-六六六115.67.8112.313.292.76.4108.29.56gamma-六六六105.89.988.35.673.28.697.56.97五氯硝基苯96.311.2105.83.972.53.289.29.58嘧霉胺89.65.9112.45.998.24.3115.21.49二嗪磷97.56.2120.311.7113.66.990.37.310乙烯菌核利108.67.895.4 10.2109.01.590.25.311甲基对硫磷110.28.989.98.4101.26.2109.42.112杀螟硫磷94.54.388.49.289.37.4107.23.213马拉硫磷107.82.1109.22.890.29.398.26.314倍硫磷91.59.1117.28.2112.54.2109.08.415毒死蜱89.23.186.43.4105.86.190.23.216对硫磷94.54.289.66.2117.88.588.34.117三氯杀螨醇88.25.2107.75.4108.27.378.97.218三唑酮103.88.2111.46.1107.63.887.38.319水胺硫磷109.29.2104.24.2 94.39.3112.77.320甲基异柳磷90.98.6109.25.2101.28.5114.38.221二甲戊乐灵89.710.2111.47.184.35.397.46.322氟虫腈96.73.2107.13.583.52.195.23.023腐霉利104.64.394.94.5112.34.2103.26.6 24丙溴磷104.12.8107.04.295.75.085.74.125p,p' -DDE107.41.486.81.184.31.597.00.926虫螨腈88.67.090.56.894.34.6106.39.827p,p' -DDD101.43.6108.24.897.35.578.41.828o,p' -DDT111.15.7107.62.1102.25.4116.05.629三唑磷109.21.088.85.096.84.789.04.430p,p' -DDT113.06.196.82.498.43.185.11.031异菌脲89.36.089.72.295.84.2110.84.732联苯菊酯112.010.0105.43.7105.86.196.43.333亚胺硫磷105.56.789.23.694.75.3108.84.134甲氰菊酯74.910.380.53.987.73.4101.812.935伏杀硫磷110.25.291.82.9101.26.0106.412.436哒螨灵97.24.291.42.395.25.7106.07.237嘧菌酯107.54.2103.8 3.999.36.5115.75.838氯氟氰菊酯107.25.9107.73.395.37.1120.68.939氯菊酯83.84.7109.83.291.86.0101.89.140氟氯氰菊酯 106.45.784.16.890.96.9112.89.741氯氰菊酯74.19.083.64.681.53.498.514.242氟氰戊菊酯85.03.883.23.280.63.2104.27.643氰戊菊酯81.88.774.03.981.93.3105.97.944氟胺氰菊酯98.92.873.24.883.55.6103.58.745苯醚甲环唑88.69.380.34.796.03.6115.810.646溴氰菊酯84.85.575.56.672.52.996.34.7 维泰克QuEChERS产品订货信息样品基质样品量提取溶剂提取包净化管EN方法蔬菜、水果、食用菌(颜色较浅的样品,如番茄、苹果、土豆、梨、甘蓝等)10.0 g10 mL乙腈4g MgSO41gNaCl1g柠檬酸钠0.5g 柠檬酸氢二钠盐包:WQ-MN40115N150 mg PSA900 mg MgSO415 mL净化管:WQ-MP09015 蔬菜、水果、食用菌(颜色较深的样品,如茄子、豆角、韭菜、芹菜等)10.0 g10 mL乙腈4g MgSO41gNaCl1g柠檬酸钠0.5g 柠檬酸氢二钠盐包:WQ-MN40115N150 mg PSA15 mg GCB885 mg MgSO4 15 mL净化管:WQ-MC309020 AOAC方法茶叶、香辛料2.0 g+10 mL水15 mL乙腈(含1%乙酸)6g MgSO41.5g NaOAc盐包:WQ-MN40115N400 mg PSA400 mg C18200 mg GCB1200 mg MgSO415 mL净化管:WQ-MG412040 谷物、油料、坚果5.0 g+10 mL水15 mL乙腈(含1%乙酸)6g MgSO41.5g NaOAc盐包:WQ-MN40115N400 mg PSA400 mg C181200 mg MgSO415 mL净化管:WQ-MC12040