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作 者:郭项雨[1] 李海玉[1] 白桦[1] 雒丽丽[1] 张武庆[1] 吕庆[1] 李丕[1] 张庆[1]
出 处:《分析试验室》2014年第8期921-923,共3页Chinese Journal of Analysis Laboratory
基 金:国家质检总局公益性行业科研专项(2012104013-9)资助
摘 要:研究并建立了洗涤用品中氮川三乙酸盐(NTA)的离子色谱测定方法。将洗涤用品样品用超纯水稀释200—500倍,置于磁力搅拌器上搅拌至完全溶解,样品提取液依次过尼龙滤膜和OnGuardII RP固相萃取柱。滤液采用离子色谱一抑制电导检测法分析测定,以Ion Pac AS11阴离子交换色谱柱分离,以KOH溶液为淋洗液进行梯度洗脱,ASRS-400阴离子型抑制电导检测,外标法定量。方法的线性范围为0.02—10μg/mL,相关系数为0.9998,对氮川三乙酸盐定量限为20mg/kg,液类洗涤用品在低、中、高3种加标水平的回收率为90.9%-103.2%,相对标准偏差为1.9%~4.1%;粉类产品在低、中、高3种加标水平的回收率为89.3%-105.1%,相对标准偏差为4.1%~6.7%;皂类产品在低、中、高3种加标水平的回收率为96.9%~115.1%,相对标准偏差为2.3%-4.2%。An ion chromatographic method was developed for the determination of nitrilotriacetic acid salt(NTA) in detergent products. The samples of detergent were dissolved in water and shaken until the samples were completely dispersed. Then the extract was filtered through nylon membrane and OnGuardlIRP solid phase extraction cartridge and detected by ion chromatography with suppressed conductivity detection. The separation was performed on an IonPac AS11 anion exchange column with gradient elution by using potassium hydroxide solution. NTA was detected using an ASRS 400 anion suppressed conductivity detector and quantified by external standard method. The linear range was 0. 02 ~ 10 p,g/mL with a correlation coefficient of 0. 9998. The limit of quantification for NTA was 20 mg/kg. The mean recoveries for liquid detergent products at three spiked levels were in the range of 90. 9% - 103.2%, with the relative standard deviations of 1.9% ~ 4. 1%. The mean recoveries for powder detergent products at three spiked levels were in the range of 89. 3% ~ 105. 1%, with the relative standard deviations of 4. 1% - 6. 7 %. in the range of 96. 9% ~ 115.1%, with the accurate, reliable and can be used to inspect The mean recoveries for soap products at three spiked levels were relative standard deviations of 2.3% -4.2%. The method is the actual detergent products.
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