离子色谱法测定口腔护理产品中的氯酸盐  

Determination of chlorate in oral care products by ion chromatography

作　　者：林立[1,2] 王琳琳[2] 孙海波[2] 杨彦丽[2] 孙继红[1] 

机构地区：[1]北京工业大学,北京100022 [2]国家食品质量安全监督检验中心,北京100094

出　　处：《中国卫生检验杂志》2014年第5期609-611,617,共4页Chinese Journal of Health Laboratory Technology

基　　金：质检公益性行业科研专项(201210215)

摘　　要：目的建立了离子色谱测定口腔护理产品中氯酸盐的方法。方法针对不同的样品基体(膏状、粉类、水剂)优化样品前处理条件,选择最优的色谱条件,包括适合的溶剂、流动相等,对方法检出限、准确度和回收率进行考查。样品经氢氧化钠水溶液超声提取,采用RP小柱去除提取液中的杂质后导入离子色谱仪测定。氯酸根和其他干扰离子被阴离子色谱柱(IonPac AS 19,50 mm×4 mm)分离,氢氧化钠淋洗液梯度洗脱,电导检测器进行定量。结果在0.05 mg/L^50.0 mg/L范围内,氯酸盐工作曲线的线性相关系数为0.9998。仪器检出限为0.010 mg/L,方法定量限为6.0 mg/kg。样品在3个水平下的加标回收率在89.6%~105.6%之间,精密度在6.3%以下。结论该方法操作简单、结果准确,适用于口腔护理产品中氯酸盐的测定。Objective A method for determination of chlorate in oral care products by ion chromatography was established. Methods The sample pretreatment method and chromatographic conditions including suitable solvent, mobile phase, the de- tection limit, accuracy and recovery test, were optimized and selected in accordance with different matrixes of samples （paste, powder, water）. The chlorate in samples was ultrasonicly extracted by sodium hydroxide solution and cleaned up on RP column for ion chromatography determination. Chlorate was separated from other interfering ions by IonPae AS 19 column （50 mm × 4 mm）, eluted by sodium hydroxide eluent and quantified by conductivity detector. Results The linear correlation coefficient of chlorate was 0. 9998 in the linear range of 0.05 mg/L - 50.0 mg/L. The instrument detection limit was 0.010 mg/L and the method quantification limit was 6.0 mg/kg. The spiked recovery at three levels was from 89.6% to 105.6%, and the relative standard deviation was below 6.3%. Conclusion The method is simple and accurate, it is suitable for determination of chlo- rate in oral care products.

关 键 词：离子色谱 电导检测 氯酸盐 口腔护理产品 

分 类 号：O657.75[理学—分析化学]