摘要
将党参样品粉碎后过0.250 mm筛,称取1.000g,加入20 mL正己烷,超声提取20min,过滤后,移取50μL滤液,加入950μL水制成1.0mL的样品溶液,迅速加入60μL邻二氯苯与200μL甲醇的混合溶液,涡旋30s,使之成为乳浊液体系,在3 500r·min~(-1)下离心5min,取下层沉积相用N2吹干,加50μL甲醇复溶后,采用气相色谱法测定其中10种有机氯类农药。在最佳试验条件下,10种有机氯农药在0.50～20.0μg·L~(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)在0.5～3.0μg·kg~(-1)之间,富集倍数在11.2～25.5之间。加标回收率在90.1%～109%之间,测定值的相对标准偏差(n=5)在1.6%～6.2%之间。
The Codonopsis Radix sample was crushed and passed through a 0.250 mm sieve.1.000 g of the sample were taken and 20 mL of n-hexane was added.After ultralsonical extraction for 20 min,the mixture was filtrated,50μL of the filtrate was taken,and 950μL of water was added to prepare 1.0 mL of sample solution.Then a mixture of 60μL of o-dichlorobenzene and 200μL of methanol were quickly added,and the mixture was vortexed for 30 sto make it a emulsion system,which was centrifuged at 3 500 r·min~(-1) for 5 min.The lower sedimentary phase was taken and dried by N2 blowing.The residue was redisolved with 50μL of methanol,and 10 organochlorine pesticides was determined by gas chromatography.Under optimized experimental conditions,linear relationships were found between peak area and corresponding mass concentration of the 10 organochlorine pesticides in the range of 0.50-20.0μg·L~(-1).The detection limits(3 S/N)were in the range of 0.5-3.0μg·kg~(-1),and the enrichment factors were in the range of 11.2-25.5.Recovery obtained by standard addition method ranged from 90.1%to109%,and the relative standard deviations(n=5)of the measured values ranged from 1.6%to 6.2%.
引文
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