Kang Qinghe, Wu Yan, Gao Kaiyang, Li Zhibin
Heilongjiang Entry-Exit Inspection and Quarantine Bureau, Harbin 150001, China.
Se Pu. 2009 Mar;27(2):181-5.
An analytical method has been developed for the determination of 28 organochlorine pesticides and pyrethroid pesticides in pine nuts. The sample was extracted With acetonitrile-water (4:1, v/v) as the extraction solution by means of high-speed homogenization. The crude extract was purified by an Aluminium-N solid phase extraction column to remove most of the fat and sterols in the sample, then on-line gel permeation chromatography-gas chromatography/ mass spectrometry (GPC-GC/MS) analysis was performed. The recoveries for the most of pesticides in the sample spiked with the standards of 0.05 mg/kg were 70%-120%, and the relative standard deviations were less than 15%. The limits of detection of 28 organochlorine pesti- and pyrethroid pesticides were 0.002-0.05 mg/kg. The linear relationship and the recovery results were satisfactory. The method is rapid, accurate, highly senstive, and can be used for the simultaneous determination of pesticide residues in pine nuts.
建立了一种测定松子中28种有机氯农药和拟除虫菊酯类农药的分析方法。以乙腈 - 水（4:1，v/v）为提取液，通过高速匀浆法提取样品。粗提物经中性氧化铝固相萃取柱净化，以去除样品中的大部分脂肪和甾醇，然后进行在线凝胶渗透色谱 - 气相色谱/质谱（GPC - GC/MS）分析。在添加0.05 mg/kg标准品的样品中，大多数农药的回收率为70% - 120%，相对标准偏差小于15%。28种有机氯农药和拟除虫菊酯类农药的检出限为0.002 - 0.05 mg/kg。线性关系和回收率结果令人满意。该方法快速、准确、灵敏度高，可用于同时测定松子中的农药残留。
