毛细管离子色谱法同时测定饮用水中痕量碘离子硫氰酸根和.docVIP

毛细管离子色谱法同时测定饮用水中痕量碘离子、硫氰酸根和草甘膦 叶明立 胡忠阳 潘广文 （戴安中国有限公司上海实验室，上海，201203） 摘要 建立了一种采用毛细管离子色谱法同时测定饮用水中痕量–、–和草甘膦的方法。样品经过0.22 μm滤膜过滤后，直接进样5μL，IonPac AS19(250×0.4mm)毛细管色谱柱分离，KOH梯度淋洗，流速10 μL/min，抑制电导检测，外标法定量。以信噪比(S/N)为3计算检出限，碘离子、硫氰酸根和草甘膦的检出限分别为0.3、0.2、0.2 ng/mL，线性范围2.0～100 μg/L，相关系数分别为0.9997、0.9998和0.9998，加标回收率为86.0%～100.6%。该方法应用于饮用水中痕量碘离子、硫氰酸根和草甘膦的测定，结果令人满意。 关键词 毛细管离子色谱；饮用水；碘离子；硫氰酸根；草甘膦 Determination of trace iodide, thiocyanate and glyphosate in drinking water by capillary ion chromatography Ye Ming-Li, Hu Zhong-Yang, Pan Guang-Wen Shanghai Lab., Dionex China Co. LTD., Shanghai 201203, China Abstract: A method was developed for the simultaneous determination of iodide, thiocyanate and glyphosate in drinking water by capillary ion chromatography (CIC). The sample was injected into CIC directly after filtrated by 0.22 μm nylon filter membrane, and then analyzed by IC. The analytical column was Dionex IonPac AS19(250×0.4mm), Gradient KOH was used as the eluent at a flow rate of 1.0 mL/min. The detection was performed by a suppressed conductive detector. The quantitive analysis of external standard calibration curves was used. The linear range of the method for iodide, thiocyanate and glyphosate were 2.0~100μg/L, the correlation coefficients were 0.9997, 0.9998 and 0.9998, and the detection limits(S/N=3) were 0.3μg/L, 0.2μg/L, 0.2μg/L respectively. The average recoveries were 86.0%~100.6%. The method has been applied to determine trace iodide, thiocyanate and glyphosate in bottled drinking water with satisfactory results. Keywords: capillary ion chromatography, drinking water, iodide, thiocyanate, glyphosate 1 引言 碘对生命体是非常重要的元素碘离子摄入量过低引起碘离子缺乏病，而碘离子摄入过量会引起高碘离子性甲亢和智力下降。饮用水中碘含量能够反映一个地区的基础碘营养水平是反映外环境碘的良好指标。硫氰酸根对人体危害很大，重复中毒可致肾功能明显损害，慢性作用，可抑制人体甲状腺聚碘功能，使人体缺碘更加严重。饮用水中硫氰酸盐主要来自工业废水由于硫氰酸根盐人体甲状腺功能，因此对其在饮用水中的存在、来源及安全阈值的研究引起了科学家的重视。草甘膦影响大脑乙酰胆胆碱酯酶的活性，降低肝糖原水平。新制定的《生活饮用水卫生标准》中, 增加了草甘膦检测项目, 给出的草甘膦的最大残留限量分别是0.7 μg/mL。 　 目前，碘离子的测定主要采用离子色谱选择性电极法高效液相色谱法、分光光度法、ICP-MS等。草甘膦的测定主要采用GC-MS, HPLC-UV紫外衍生法