Department of Chemistry, University of Cincinnati, Cincinnati, OH 45221-0172, USA.
Talanta. 2002 Nov 12;58(5):899-907. doi: 10.1016/s0039-9140(02)00404-6.
In this study, a rapid and sensitive high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) determination of primary As species in fish tissues and urine is reported. The separation was achieved on an Altima C18 column with a mobile phase containing citric acid and hexanesulfonic acid (pH 4.5). As(V), monomethylarsonic acid (MMA), As(III), dimethylarsinic acid (DMA) and arsenobetaine (AsB) were separated in less than 4 min with retention times of 83, 99, 130, 166 and 208 s, respectively. This separation of five species in less than 4 min should be attractive to those interested in As speciation. The quantification limits were 44, 56, 94, 64, 66 ng l(-1) and the relative standard deviations (R.S.D.) for day-to-day injections of As at 2 mug l(-1) were 2.0, 3.1, 2.4, 3.8 and 4.0%. The procedure was tested using two reference materials (DORM-2 dogfish muscle tissue, NIST SRM 2670 Freeze-dried Urine, normal level) and then applied to real-world samples. The results obtained demonstrate the suitability of the procedure for screening and quantification at physiological levels of primary As species in biological samples.
本研究报告了一种快速灵敏的高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS)测定鱼组织和尿液中初级砷形态的方法。该分离在 Altima C18 柱上进行,流动相含有柠檬酸和己烷磺酸(pH 4.5)。As(V)、一甲基砷酸(MMA)、As(III)、二甲基砷酸(DMA)和砷甜菜碱(AsB)在不到 4 分钟的时间内得到分离,保留时间分别为 83、99、130、166 和 208 s。这种在不到 4 分钟内分离五种形态的方法应该会吸引那些对砷形态感兴趣的人。定量限分别为 44、56、94、64、66ng l(-1),在 2μg l(-1)的 As 日内注射的相对标准偏差(R.S.D.)为 2.0、3.1、2.4、3.8 和 4.0%。该方法使用两种参考材料(DORM-2 鲨鱼肌肉组织、NIST SRM 2670 冷冻尿液、正常水平)进行了测试,然后应用于实际样品。结果表明,该方法适用于在生理水平下筛选和定量生物样品中的初级砷形态。