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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-抑制电导检测法分析测定,以IonPac 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20 mg/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%。
A method for the determination of nitrilotriacetate (NTA) in detergents by ion chromatography has been studied and established. Dilute the detergent sample 200 to 500 times with ultrapure water, place it on a magnetic stirrer and stir until it completely dissolves. The sample extract passes through a nylon filter and an OnGuard II RP solid phase extraction cartridge. The filtrate was analyzed by ion chromatography-suppressed conductivity detection, separated by IonPac AS11 anion exchange column and eluted with KOH solution. ASRS-400 anion-suppressed conductivity detection and external standard method. The linear range of the method was 0.02 ~ 10μg / mL, the correlation coefficient was 0.9998, the limit of quantification of nitrilotriacetate was 20 mg / kg, the recoveries of liquid detergent at low, medium and high levels were The relative standard deviations (RSDs) ranged from 90.9% to 103.2% with relative standard deviations from 1.9% to 4.1%. The recoveries of the spiked products were 89.3% -105.1% at low, medium and high spiked levels with relative standard deviations of 4.1% -6.7%. The recovery rates of soap products at low, medium and high levels were 96.9% ~ 115.1% and the relative standard deviations were 2.3% ~ 4.2%.