竹笋、油茶中 8 种有机氯和 3 种拟除虫菊酯农药残留的测定气相色谱法

竹笋、油茶中8种有机氯和3种拟除虫菊酯农药残留的测定气相色谱法p,p'-DDE、o,p'-DDT、p,p'-DDD、p,p'-农药残留的气相色谱的检测方法。本标准方法检出限为:竹笋:0.0009~0.0046mg/kg，油茶:0.0002~0.0010mg/kg，测下列文件中的条款通过本标准的引用而成为本标准的条款。凡是注明日期的引用除另有规定外，本方法所用试剂均为分析纯，水为GB/T6682规定的一级水。4.2标准贮备液：8种有机氯：ρ=1000μg/mL、联苯菊酯ρ=1000μg4.3标准使用液：分别移取8种有机氯、联苯菊酯、甲氰菊酯、氯氟氰菊酯1.0mL4.3.1混合标准中间液（10μg/mL）：分别移取8种有机氯、联苯菊酯、甲氰菊酯、氯氟氰菊酯1.0mL置于10mL容量瓶中，用正己烷定容并混匀，配制浓度均为10）：5.1气相色谱仪，配有电子捕获检测器（ECD）。5.2色谱柱：石英毛细管柱，30m×0.32mm，内涂5%苯基甲基聚硅氧烷，膜厚5.3振荡器。5.4离心机：转速≥10000r/min。5.5电子天平：精度0.01mg和0.01g。5.6粉碎机。5.7涡旋混合器。准确称取10.0g（精确至0.01g）试样置于50mL离心管中油茶先加入5mL），），硫酸镁（4.1.2）和1g氯化钠（4.1.3），混匀，以5000r/min离心5min使乙腈和移取1.5mL竹笋上层提取液置于装有200mg无水硫酸镁（4.1.2）和100mgPSA和30mg石墨化碳黑（4.1.4）的离心管中，涡旋混合30s，以5000r/min离心机离），a)色谱柱：石英毛细管柱，30m×0.32mm，内涂5%苯基甲基聚硅氧烷，膜厚按照与校准曲线建立（7.2）相同的仪器参考条件按照与试样测定（6.2）相同的步骤进行），试样中被测农药残留量以质量分数"结果按式（1）计算："—试样中各待测组分的含量，单位为毫克每千克（mg/kg）；V—试样溶液最终定容体积，单位为毫升（f—试样制备过程中的稀释倍数；在重复性条件下获得的两次独立测定结果的绝对差值不得超过算术平均值的（色谱参考图）1—α-六六六；2—γ-六六六；3—β-六六六；4—δ-六六六；5—p,p'-DDE；6—o,p'-DDT；7—p,p'-DDD；8—p,p'-DDT；9—联苯菊酯；10—甲氰菊酯；11—氯氟氰菊酯图111种农药标准工作溶液的气相色谱参考图（资料性附录）检出限、精密度和正确度附录B.1方法检出限序号样品名称化合物名称检出限（mg/kg）测定下限（mg/kg）1α-六六六0.00140.00562γ-六六六0.00090.00363β-六六六0.00150.00604δ-六六六0.00170.00685p,p'-DDE0.00160.00646o,p'-DDT0.00170.00687p,p'-DDD0.00230.00928p,p'-DDT0.00210.00849联苯菊酯0.00460.0180甲氰菊酯0.00090.0036氯氟氰菊酯0.00190.0076油茶α-六六六0.00020.0008γ-六六六0.00030.0012β-六六六0.00030.0012δ-六六六0.00100.0040p,p'-DDE0.00050.0020o,p'-DDT0.00030.0012p,p'-DDD0.00020.0008p,p'-DDT0.00050.002020联苯菊酯0.00050.002021甲氰菊酯0.00030.001222氯氟氰菊酯0.00050.0020附录B.2方法精密度序号化合物名称加标浓度(μg/mL）平均值(μg/mL）相对标准偏差范重复性限r(μg/mL)1α-六六六0.050.043.44%～3.82%0.00420.50.473.11%～3.38%0.0430.943.51%～3.84%0.14γ-六六六0.050.05512.23%～2.37%0.00450.50.50111.31%～1.36%0.0260.96631.82%～1.92%0.17β-六六六0.050.04153.98%～4.51%0.00580.50.47593.93%～4.34%0.0690.94574.23%～4.70%0.1δ-六六六0.050.03629.10%～12.0%0.010.50.497211.0%～14.7%0.20.99886.83%～7.98%0.2p,p'-DDE0.050.04443.84%～4.26%0.0050.50.48183.56%～3.96%0.050.95822.64%～2.84%0.1o,p'-DDT0.050.04304.79%～5.55%0.0060.50.48413.98%～4.42%0.060.94214.49%～5.01%0.1p,p'-DDD0.050.04532.56%～2.73%0.003200.50.46612.81%～3.04%0.04210.93662.59%～2.77%0.122p,p'-DDT0.050.03875.03%～5.90%0.006230.50.44157.21%～8.64%0.1240.93173.99%～4.41%0.125联苯菊酯0.050.06161.93%～2.04%0.003260.50.54361.14%～1.17%0.02271.01911.66%～1.75%0.0528甲氰菊酯0.050.06262.11%～2.25%0.004290.50.53251.61%～1.69%0.02301.05012.26%～2.41%0.131氯氟氰菊酯0.050.04206.08%～7.29%0.008320.50.48745.93%～6.82%0.09330.98176.00%～7.06%0.2附录B.3竹笋加标实验结果序号化合物名称加标浓度（mg/kg）加标回收率范围(％)P1α-六六六0.0584.1～110.520.599.0～105.8394.3～97.696.44γ-六六六0.0578.2～93.088.450.5107.6～115.2673.7～76.075.37β-六六六0.0581.0～108.080.5104.3～111.2993.7～97.996.0δ-六六六0.0587.3～116.90.5102.2～118.985.6～95.788.8p,p'-DDE0.0564.4～86.074.80.589.4～104.499.499.5～103.1o,p'-DDT0.0563.4～100.485.00.599.7～110.492.5～96.594.9p,p'-DDD0.0566.0～108.393.2200.598.7～105.72196.7～101.799.922p,p'-DDT0.0561.0～99.385.4230.598.0～105.52493.6～98.496.225联苯菊酯0.0566.0～134.7260.568.6～116.286.927105.2～108.828甲氰菊酯0.0593.1～106.799.7290.530104.7～108.831氯氟氰菊酯0.0571.4～104.591.2320.573.5～111.186.43399.4～104.4附录B.4油茶加标实验结果序号化合物名称加标浓度（mg/kg）加标回收率范围(％)P1α-六六六0.0589.5～94.091.620.592.0～105.9390.8～96.793.94γ-六六六0.05113.5～119.650.597.4～108.0671.3～74.572.67β-六六六0.0589.9～95.692.180.5105.2～114.3995.6～99.697.2δ-六六六0.0571.0～87.474.20.597.5～105.981.5～93.888.7p,p'-DDE0.0587.6～95.793.80.566.5～103.188.589.7～96.092.7o,p'-DDT0.0598.7～103.60.593.4～104.498.890.6～94.492.4p,p'-DDD0.0572.0～75.674.0200.571.9～101.488.82191.2～95.393.022p,p'-DDT0.0573.0～82.075.4230.574.