On the basis of GB/T 19857-2005,the aim of this research is to optimize the methods of extracting and concentrating LG and LMG from fishery products detecti by HPLC-UV.Some factors having effect on recovery rate have been studied,such as alumina,solution of hydroxylamine hydrochloride,solution of p-toluene sulfonic acid,enrichment and purification methods,sodium chloride and buffer solution of ammonium acetate.The results of this investigation show that the specimen with about 5 g have been extraced by acetonitrile on the condition when the dosage of solution of hydroxylamine hydrochloride is 2 mL,as well as solution of p-toluene sulfonic acid (1.0 mL/L) is 1 mL,buffer solution of ammonium acetate (20％) is 2 mL,acidic alumina should be 8 g and sodium chloride should be 2 g.The specimens have been successively separated and purified,while clear liquid in the upper level has been evaporated by rotating.It can be expected that the recovery would reach its peak value which MG is 95.6％ as well as LMG is 101.2％.In addition,this is a high-recovery method which has simple pretreatment,and is applicable for quickly and accurate determination of large number of samples.%在GB/T 19857-2005基础上,建立一种水产品中残留的孔雀石绿和隐形孔雀石绿的提取及富集的优化方法,并用高效液相色谱-紫外检测器的方法对目标物进行检测.考察了氧化铝、盐酸羟胺溶液和对-甲苯磺酸钠溶液、氯化钠、乙酸胺溶液及富集净化的方法等因素对水产品中孔雀石绿和隐形孔雀石绿的回收率影响.结果表明,5 g左右样品在用乙腈提取时,需加入2 mL质量分数为20％的盐酸羟胺溶液,1 mL浓度为1.0 mol/L的对-甲苯磺酸钠溶液,2 mL浓度为0.1 mol/L的乙酸胺溶液(用冰乙酸调节ptH值至4.5),8 g酸性氧化铝,2 g氯化钠;采用此法目标物的回收率最高,其中孔雀石绿可达95.6％,隐形孔雀石绿可达101.2％.该法具有操作简单、回收率高、快速大批量处理等优点.
展开▼
