水产品中甲基汞测定的液相色谱-原子荧光光谱联用方法的改进

色谱 , 2011, 29(7): 667-672. doi: 10.3724/SP.J.1123.2011.00667

水产品中甲基汞测定的液相色谱-原子荧光光谱联用方法的改进

尚晓虹 ^1, , 赵云峰 ^2, , 张磊 ^3, , 李筱薇 ^4, , 吴永宁 ^5,

1.中国疾病预防控制中心营养与食品安全所,北京,100021

2.中国疾病预防控制中心营养与食品安全所,北京,100021

3.中国疾病预防控制中心营养与食品安全所,北京,100021

4.中国疾病预防控制中心营养与食品安全所,北京,100021

5.中国疾病预防控制中心营养与食品安全所,北京,100021

基金项目: 卫生行业公益项目(200902009) "十一五"国家科技支撑计划项目(2006BAK02A10)

关键词：液相色谱 , 原子荧光光谱 , 甲基汞 , 形态分析 , 水产品

Improvement of the method for methylmercury determination in aquatic products using liquid chromatography online coupled with atomic fluorescence spectrometry

对本实验室前期建立的食品中甲基汞的液相色谱-原子荧光光谱联用测定方法进行了改进.采用无毒的半胱氨酸代替有毒试剂巯基乙醇作为流动相中的配位剂,流动相组成为5%(v/v)乙腈-1 g/L半胱氨酸-50 mmol/L乙酸铵水溶液,使汞化合物分离时间缩短至8 min.在优化条件下,甲基汞标准曲线的线性范围为1～50 μg/L,检出限(S/V=3)为0/3μg/L.采用超声波辅助5 mol/L HCl提取样品中的甲基汞,提取液经C<,18>固相萃取小柱净化后进样.鱼、虾、贝等不同种类水产动物样品以及水产类膳食样品的甲基汞加标回收率为89%～112%.对标准参考物质NIST1566b、BCR464和GBW10029以及英国食品分析水平评估计划(Food Analysis Performance Assess-ment Scheme,FAPAS)的罐装鱼肉样品(样品编号07115)的测定结果与参考物定值相符,验证了该方法的可靠性与准确性.本方法可满足食品中甲基汞检测的需要.

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