论文部分内容阅读
[目的]目前国内关于抗倒胺的检测方法只有SN 0532—1996《出口粮谷中抗倒胺残留量检验方法》。该方法前处理步骤操作繁琐且使用大量毒性较高的溶剂。通过优化溶剂、简化前处理等建立了一种用气相色谱仪分析大米中抗倒胺残留量的分析方法。样品经乙腈提取,正己烷去脂和弗罗里硅土柱净化,提取净化液经氯乙酰化后,用配有电子俘获检测器的气相色谱仪进行测定。[结果]建立的残留分析方法在0.02~0.50 mg/kg水平的平均添加回收率为86.4%~98.0%,相对标准偏差为4.0%~7.1%,抗倒胺最小检出量为2×10-10 g,最低检测质量分数为0.01 mg/kg。[结论]方法准确可靠,能够满足国外对大米抗倒胺残留限量的要求。
[Objective] At present, there are only SN 0532-1996 Test Methods for Anti-Amine Residues in Export Grains in China. The method pretreatment steps are cumbersome and use a large amount of toxic solvents. By optimizing the solvent and simplifying the pretreatment, an analytical method for the analysis of anti-amidine residue in rice by gas chromatograph was established. The sample was extracted with acetonitrile, degreased with n-hexane and purified with Florisil, and the extract was purified by chloroacetylation using a gas chromatograph equipped with an electron capture detector. [Result] The average recoveries of the residue analysis method established in the range of 0.02-0.50 mg / kg were 86.4% -98.0%, the relative standard deviations were 4.0% -7.1%, and the minimum detectable amount of anti-melamine was 2 × 10- 10 g, the lowest detection mass fraction of 0.01 mg / kg. [Conclusion] The method was accurate and reliable, which could meet the foreign requirements of rice anti-amines residue limit.