Ion-pairing reversed-phase chromatography coupled to inductivelycoupled plasma mass spectrometry as a tool to determine mercurialspecies in freshwater fish
Ion-pairing reversed-phase chromatography coupled to inductivelycoupled plasma mass spectrometry as a tool to determine mercurialspecies in freshwater fish
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离子对反相色谱法与电感耦合等离子体质谱联用作为测定淡水鱼中汞种类的工具
DOI：
10.1016/j.chroma.2017.11.029
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发表时间：
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影响因子：
4.1
通讯作者：
Jinhua Liu
中科院分区：
文献类型：
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作者：
Heyong Cheng;Xiaopan Chen;Lihuan Shen;Yuanchao Wang;Zigang Xu;Jinhua Liu
大多数分析界都集中在反相高效液相色谱法（RP-HPLC）上，该方法采用由高盐和适量有机溶剂组成的流动相进行汞形态分析。本研究采用离子配对RP-HPLC -电感耦合等离子体质谱（ICP-MS）检测，在低盐条件下快速分析汞的形态，以实现绿色分析化学。分别使用带正电和负电的离子配对试剂（四丁基氢氧化铵-TBAH和十二烷基苯磺酸钠-SDBS），在流动相中分别加入3-巯基-1-丙磺酸钠（MPS）和l-半胱氨酸（Cys），将汞转化为带负电和正电的hg配合物，以获得较好的分辨率。添加苯丙氨酸也被用于与短C18guard柱结合的快速基线分离。最佳流动相为2.0 mM SDBS + 2.0 mM Cys + 1.0 mM Phe （pH 3.0）和4.0 mM TBAH + 2.0 mM MPS + 2.0 mM Phe (pH 6.0)，均可在两个连续的12.5 mM c18柱上实现无机汞（Hg2+）、甲基汞（MeHg）、乙基汞（EtHg）和苯基汞（PhHg）的基线分离。由于前者的分离时间较短（3.0 min），因此选择前者作为淡水鱼体内汞形成的流动相。Hg2+的检出限为0.015，MeHg的检出限为0.014，EtHg的检出限为0.028，PhHg的检出限为0.042 μg L - 1，峰高和面积的精度为1.0 ~ 2.8% （5.0 μg L - 1 -混合物标准）。鱼组织（GBW 10029）和金枪鱼（BCR-463）认证标准物质中MeHg和总汞的测定值与认证值吻合良好，回收率在91 ~ 106%之间，证明了该方法具有良好的准确性。在淡水鱼中的应用表明了其在常规分析中的潜力，其中MeHg在3.7 ~ 20.3 μ kg−1之间为优势种。
Most of analytical community is focused on reversed phase high performance liquid chromatography (RP-HPLC) for mercury speciation by employing mobile phases comprising of high salts and moderate amounts of organic solvents. This study aims at rapid mercury speciation analysis by ion-pairing RP-HPLC with inductively coupled plasma mass spectrometry (ICP-MS) detection only using low salts for the sake of green analytical chemistry. Two ion-pairing HPLC methods were developed on individual usage of positively and negatively charged ion-pairing reagents (tetrabutylammonium hydroxide –TBAH and sodium dodecylbenzene sulfonate –SDBS), where sodium 3-mercapto-1-propysulfonate (MPS) andl-cysteine (Cys) were individually added in mobile phases to transform mercury species into negative and positive Hg-complexes for good resolution. Addition of phenylalanine was also utilized for rapid baseline separation in combination of short C18guard columns. Optimum mobile phases of 2.0 mM SDBS + 2.0 mM Cys + 1.0 mM Phe (pH 3.0) and 4.0 mM TBAH + 2.0 mM MPS + 2.0 mM Phe (pH 6.0) both achieved baseline separation of inorganic mercury (Hg2+), methylmercury (MeHg), ethylmercury (EtHg) and phenylmercury (PhHg) on two consecutive 12.5-mm C18columns. The former mobile phase was selected for mercury speciation in freshwater fish because of short separation time (3.0 min). Detection limits of 0.015 for Hg2+, 0.014 for MeHg, 0.028 for EtHg and 0.042 μg L−1for PhHg were obtained along with satisfactory precisions of peak height and area (1.0-2.8% for 5.0 μg L−1Hg-mixture standard). Good accordance of determined values of MeHg and total mercury in certified reference materials of fish tissue (GBW 10029) and tuna fish (BCR-463) with certified values as well as good recoveries (91–106%) proved good accuracy of the proposed method. An example application to freshwater fish indicated its potential in routine analysis, where MeHg was presented at 3.7–20.3 μg kg−1as the dominate species.