气相色谱检测啤酒中十六种有机磷农药残留方法的建立

建立啤酒中16种有机磷农药残留的气相色谱检测方法,量取试样5 mL,外部加标后加1%酸化乙腈10 mL提取,加氯化钠分层后取乙腈层过有机相尼龙针式滤器,进气相色谱氢火焰光度检测器(Flame Photometric Detector,FPD)测定。结果表明,16种有机磷在0.03、0.05、0.08 mg/L三种不同加标浓度下的回收率在72.33%~113.00%,相对标准偏差(Relative Standard Deviation,RSD)在0.52%~9.92%;检出限0.0040~0.0190 mg/kg,定量限0.0132~0.0627 mg/L,线性范围0.01~10.0 mg/L;该检测方法前处理操作简捷、试剂消耗量少、回收率高、检测结果稳定,可满足市售多种品类啤酒中以上16种有机磷农药残留的检测需求。

Establishment of Gas Chromatographic (GC) Method for the Detection of 16 Kinds of Organophosphorus (OPs) Pesticide Residues in Beer

A GC method for the determination of 16 kinds of OPs pesticide residues in beer was established. The samples were (5 mL), extracted with 1% acidified acetonitrile at 10 mL with the addition of external reference material, stratified with NaCl, and then the acetonitrile layer was taken through the organic phase nylon needle filter for determination by GC FPD detector. The results showed that the recovery rate of 16 kinds of OPs at 0.03, 0.05 and 0.08 mg/L were 72.33%~113.00%, the relative standard deviation (RSD) was 0.52%~9.92%. The detection limit was 0.0040~0.0190 mg/kg, the quantitative limit was 0.0132~0.0627 mg/L, and the linear range was 0.01~10.0 mg/L. The pretreatment operation is simple, the consumption of reagents is littleness, the recovery rate is high, and the detection results are stable. It can satisfy the testing requirements of 16 kinds of OPs pesticide residues in various beers on the market.