高效液相色谱-电感耦合等离子体质谱法和高效液相色谱-氢化物发生原子吸收光谱法测定鱼组织和沉积物中的甲基汞（I）和汞（II）。
Measurement of methyl mercury (I) and mercury (II) in fish tissues and sediments by HPLC-ICPMS and HPLC-HGAAS.
机构信息
Ecochemistry Laboratory, Institute for Applied Ecology, University of Canberra, Bruce, ACT 2601, Australia.
出版信息
Talanta. 2011 Jul 15;85(1):49-55. doi: 10.1016/j.talanta.2011.03.022. Epub 2011 Apr 1.
A procedure for the extraction and determination of methyl mercury and mercury (II) in fish muscle tissues and sediment samples is presented. The procedure involves extraction with 5% (v/v) 2-mercaptoethanol, separation and determination of mercury species by HPLC-ICPMS using a Perkin-Elmer 3 μm C8 (33 mm×3 mm) column and a mobile phase 3 containing 0.5% (v/v) 2-mercaptoethanol and 5% (v/v) CH(3)OH (pH 5.5) at a flow rate 1.5 ml min(-1) and a temperature of 25°C. Calibration curves for methyl mercury (I) and mercury (II) standards were linear in the range of 0-100 μgl(-1) (r(2)=0.9990 and r(2)=0.9995 respectively). The lowest measurable mercury was 0.4 μgl(-1) which corresponds to 0.01 μgg(-1) in fish tissues and sediments. Methyl mercury concentrations measured in biological certified reference materials, NRCC DORM - 2 Dogfish muscle (4.4±0.8 μgg(-1)), NRCC Dolt - 3 Dogfish liver (1.55±0.09 μgg(-1)), NIST RM 50 Albacore Tuna (0.89±0.08 μgg(-1)) and IRMM IMEP-20 Tuna fish (3.6±0.6 μgg(-1)) were in agreement with the certified value (4.47±0.32μgg(-1), 1.59±0.12 μgg(-1), 0.87±0.03 μgg(-1), 4.24±0.27 μgg(-1) respectively). For the sediment reference material ERM CC 580, a methyl mercury concentration of 0.070±0.002 μgg(-1) was measured which corresponds to an extraction efficiency of 92±3% of certified values (0.076±0.04 μgg(-1)) but within the range of published values (0.040-0.084 μgg(-1); mean±s.d.: 0.073±0.05 μgg(-1), n=40) for this material. The extraction procedure for the fish tissues was also compared against an enzymatic extraction using Protease type XIV that has been previously published and similar results were obtained. The use of HPLC-HGAAS with a Phenomenox 5 μm Luna C18 (250 mm×4.6 mm) column and a mobile phase containing 0.06 moll(-1) ammonium acetate (Merck Pty Limited, Australia) in 5% (v/v) methanol and 0.1% (w/v) l-cysteine at 25°C was evaluated as a complementary alternative to HPLC-ICPMS for the measurement of mercury species in fish tissues. The lowest measurable mercury concentration was 2 μgl(-1) and this corresponds to 0.1 μgg(-1) in fish tissues. Analysis of enzymatic extracts analysed by HPLC-HGAAS and HPLC-ICPMS gave equivalent results.
本文介绍了一种从鱼类肌肉组织和沉积物样品中提取和测定甲基汞和汞（II）的方法。该方法采用 5%（v/v）2-巯基乙醇进行提取，然后通过高效液相色谱-电感耦合等离子体质谱（HPLC-ICPMS）分离和测定汞形态，使用 Perkin-Elmer 3 μm C8（33mm×3mm）柱和流动相 3，其中含有 0.5%（v/v）2-巯基乙醇和 5%（v/v）甲醇（pH5.5），流速为 1.5ml/min，温度为 25°C。甲基汞（I）和汞（II）标准品的校准曲线在 0-100μgl（-1）范围内呈线性（r（2）分别为 0.9990 和 0.9995）。最低可测汞为 0.4μgl（-1），相当于鱼类组织和沉积物中的 0.01μgg（-1）。在生物标准参考物质中的甲基汞浓度测量值与认证值一致，NRCC DORM-2 狗鱼肌肉（4.4±0.8μgg（-1））、NRCC Dolt-3 狗鱼肝（1.55±0.09μgg（-1））、NIST RM 50 金枪鱼（0.89±0.08μgg（-1））和 IRMM IMEP-20 金枪鱼（3.6±0.6μgg（-1））。对于沉积物标准物质 ERM CC 580，测量到的甲基汞浓度为 0.070±0.002μgg（-1），相当于认证值的 92±3%（0.076±0.04μgg（-1）），但在该物质的已发表值范围内（0.040-0.084μgg（-1）；平均值±s.d.：0.073±0.05μgg（-1），n=40）。与先前已发表的使用蛋白酶 XIV 进行的酶提取相比，还比较了鱼类组织的提取程序，得到了相似的结果。使用高效液相色谱-氢化物发生原子吸收光谱法（HPLC-HGAAS），采用 Phenomenox 5μm Luna C18（250mm×4.6mm）柱，流动相含有 0.06mol/L 乙酸铵（澳大利亚默克公司）、5%（v/v）甲醇和 0.1%（w/v）L-半胱氨酸，在 25°C 下作为 HPLC-ICPMS 的补充替代方法，用于测量鱼类组织中的汞形态。最低可测汞浓度为 2μgl（-1），相当于鱼类组织中的 0.1μgg（-1）。用 HPLC-HGAAS 和 HPLC-ICPMS 分析酶提取物得到了等效的结果。
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