论文部分内容阅读
建立了高效液相色谱-荧光检测器(HPLC-FLD)检测水产品中乙氧喹啉残留量的方法。试样加入碳酸钠溶液和丙酮振荡提取后,用正己烷进行液-液萃取分配,取正己烷层浓缩近干后,再用乙腈溶解,溶解液经氧化铝固相萃取小柱净化,收集所有过滤液,氮气吹干定容后,用配有荧光检测器的高效液相色谱仪测定,外标法定量。结果表明,乙氧喹啉在0.01～10μg/mL的范围内呈良好的线性关系,相关系数为0.9997。在添加浓度为0.01、0.02、0.5、1.0和2.0mg/kg5个添加水平下,样品的平均回收率为71.2%～94.7%,相对标准偏差小于10%;方法的测定低限为0.01mg/kg。该方法操作简便、净化效果好、灵敏度高,适用于水产品中乙氧喹啉的检测。
A method for the determination of ethoxyquin residues in aquatic products by HPLC-FLD was established. The sample was added sodium carbonate solution and acetone oscillation extraction, the liquid-liquid extraction with n-hexane, the n-hexane layer was concentrated and nearly dry, and then dissolved in acetonitrile, the solution was purified by alumina solid-phase extraction cartridge to collect all After the filtrate was filtered and dried with nitrogen, the volume of the filtrate was measured by a high performance liquid chromatograph equipped with a fluorescence detector and quantified by an external standard method. The results showed that ethoxyquin had a good linearity in the range of 0.01 ~ 10μg / mL with a correlation coefficient of 0.9997. The average recoveries of the samples were 71.2% ~ 94.7% with the relative standard deviations of less than 10% at the five addition levels of 0.01, 0.02, 0.5, 1.0 and 2.0 mg / kg; the lower limit of determination was 0.01 mg / kg . The method has the advantages of simple operation, good purification effect and high sensitivity, and is suitable for the detection of ethoxyquin in aquatic products.