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目的建立高效液相色谱-电感耦合等离子体质谱法(high performance liquid chromatography-inductively coupled plasma-mass spectrometry,HPLC-ICP-MS)测定东海乌参样品中的二价汞、甲基汞、乙基汞和苯基汞4种汞形态的含量。方法样品经25%KOH微波萃取1 h,采用Agilent Zorbax Plus C_(18)色谱柱分离,以10 mmol/L醋酸铵+0.12%L-半胱氨酸缓冲盐及2%甲醇作为流动相进行梯度洗脱,采用ICP-MS进行检测。结果二价汞、甲基汞、乙基汞和苯基汞在10 min内完成分离,检出限分别为0.8、0.2、0.2和0.8 ng/m L;在0.10、0.20和0.40mg/kg 3个加标水平下,4种汞化合物的回收率为78.1%~105.8%,相对标准偏差为5.3%~8.2%。结论本方法简便、快速、准确,可适用于汞形态的分析。
Objective To establish a HPLC-ICP-MS for the determination of bivalent mercury, methylmercury, ethylmercury And phenyl mercury four kinds of mercury content. Methods The samples were extracted with 25% KOH by microwave for 1 h and separated on an Agilent Zorbax Plus C 18 column. The gradient of 10 mmol / L ammonium acetate + 0.12% L-cysteine buffer and 2% methanol as the mobile phase Elution was detected by ICP-MS. Results The separation of bivalent mercury, methylmercury, ethylmercury and phenylmercury was completed within 10 min with detection limits of 0.8, 0.2, 0.2 and 0.8 ng / m L, respectively; at 0.10, 0.20 and 0.40 mg / kg 3 Under the spiked levels, the recoveries of four mercury compounds ranged from 78.1% to 105.8% with relative standard deviations of 5.3% -8.2%. Conclusion The method is simple, rapid and accurate and can be applied to the analysis of mercury speciation.