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    气相色谱-电子捕获检测器快速测定水产品中多种农药及兽药残留

    Rapid Determination of Pesticide and Veterinary Drug Residues in Aquatic Products by Gas Chromatography-Electro Capture Detector

    • 摘要: 称取2.000 g样品,加入含0.2%(φ)甲酸的乙腈(85+15)溶液10 mL,涡旋混合30 s,振荡提取30 min,以10 000 r·min-1转速离心5 min,取上清液。用2 mL的含0.2%(φ)甲酸的乙腈(85+15)溶液活化Oasis PRiME HLB小柱后,将上述上清液全部通过Oasis PRiME HLB小柱并收集滤液,于50℃水浴下氮吹至干,加入100 μL衍生化试剂N,O-双(三甲基硅烷基)三氟乙酰胺-三甲基氯硅烷(质量比为99:1),涡旋10 s,于65℃恒温反应30 min后,于50℃水浴下氮吹至干,用正己烷定容至1.0 mL,以DB-5/DB-35色谱柱(30 m×0.25 mm,0.25 μm)分离11种拟除虫菊酯类农药和3种氯霉素类兽药,采用电子捕获检测器。11种农药的线性范围为0.10~0.80 mg·L-1,3种兽药的线性范围为5.0~40 mg·L-1,检出限(3S/N)在0.000 1~0.008 0 μg·g-1之间。加标回收率为85.6%~119%,测定值的相对标准偏差(n=6)不大于9.0%。

       

      Abstract: 10 mL of acetonitrile (85+15) solution containing 0.2% (φ) formic acid was added to 2.000 g of the sample. The mixture was vortexed for 30 s, extracted by oscillation for 30 min, and centrifuged at 10 000 r·min-1 for 5 min, and the supernatant was taken. After the Oasis PRiME HLB cartridge was activated with 2 mL of acetonitrile (85+15) solution containing 0.2% (φ) formic acid, the supernatant was passed through the Oasis PRiME HLB cartridge and the filtrate was collected and dried by N2-blowing in a water bath at 50℃. Then 100 μL of derivatization reagentN,O-bis(trimethylsilyl) trifluoroacetamide-trimethylchlorosilane (mass ration of 99:1) was added to the resdiue, and the mixture was vortexed for 10 s and let react at a constant temperature of 65℃ for 30 min. After the mixture was dried by N2-blowing in a water bath at 50℃, and the residue was made up to 1.0 mL with n-hexane. 11 pyrethroid pesticides and 3 chloramphenicol veterinary drugs were separated on a DB-5/DB-35 column (30 m×0.25 mm, 0.25 μm) and determined by using an electron capture detector. The linear range of 11 pesticides was 0.10-0.80 mg·L-1, the linear range of 3 veterinary drugs was 5.0-40 mg·L-1, and the detection limits (3S/N) were between 0.000 1-0.008 0 μg·g-1. Values of recovery obtained by standard addition method ranged from 85.6% to 119%, and RSDs (n=6) were not more than 9.0%.

       

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