摘要
建立了一种离子色谱测定洗涤剂样品中9种螯合剂含量的分析方法。洗涤剂样品经去离子水稀释,IC-RP固相萃取小柱净化后,选择高容量的Dionex IonPac^(TM)AS11-HC型阴离子色谱柱进行分离,以自动淋洗液发生器电解产生的高纯KOH溶液为流动相进行梯度淋洗,流速1.0 mL/min,采用高压离子色谱仪电导检测器进行测定,外标法定量。结果显示,葡萄糖酸钠、甲基甘氨酸二乙酸三钠、次氮基三乙酸、羟基乙叉二膦酸、柠檬酸钠、焦磷酸钠、谷氨酸二乙酸四钠和三聚磷酸钠在1~200 mg/L范围内、乙二胺四乙酸二钠(EDTA-2Na)在50~500 mg/L范围内线性良好,相关系数(r)>0.999。EDTA-2Na的检出限(S/N=3)为12.5 mg/L,定量下限(S/N=10)为40 mg/L;其余8种螯合剂的检出限为0.02~0.07 mg/L,定量下限为0.06~0.25 mg/L。9种螯合剂在低、中、高3个加标水平下的平均回收率为92.7%~106%,相对标准偏差(RSD)为1.0%~7.9%,均满足检测要求。该方法无需衍生化处理,前处理简单,测定快速,结果准确,灵敏度高,适用于洗涤剂样品中9种螯合剂的定量分析,为洗涤用品的质量评价提供了强有力的方法支持。
A novel method based on ion chromatography was established for the determination of nine chelators in detergent samples.The samples were firstly diluted with deionized water,then purified with IC-RP solid phase extraction columns to eliminate the damage of surfactants in the detergent samples to the chromatographic column,followed by separation on a Dionex IonPac^(TM) AS11-HC an⁃ion analysis column with high capacity,using a gradient elution with a high purity of potassium hy⁃droxide(KOH)aqueous solution as the eluent at a flow rate of 1.0 mL/min,which was produced by an automatic generator,and finally detected by Thermo Fisher Intergrion high pressure ion chromato⁃graph with conductivity detector,and quantified using an external standard method.Sodium gluco⁃nate(GNa),trisodium methylglycine diacetate(MGDA),nitrous triacetic acid(NTA),hydroxyl ethylidene diphosphonic acid(HEDP),sodium citrate(CANa),sodium pyrophosphate(TSPP),tetrasodium glutamate diacetate(GLDA)and sodium tripolyphosphate(STPP)showed good linear re⁃lationships within the range of 1-200 mg/L.Disodium ethylenediamine tetraacetate(EDTA-2Na)showed a good linear relationship in the range of 50-500 mg/L.The correlation coefficients(r)were greater than 0.999.The limit of detection(S/N=3)and limit of quantitation(S/N=10)for EDTA-2Na were 12.5 mg/L and 40 mg/L,respectively.The limits of detection and the limits of quantita⁃tion for the other eight chelators were in the range of 0.02-0.07 mg/L and 0.06-0.25 mg/L,re⁃spectively.The average spiked recoveries at high,medium and low three levels ranged from 92.7%to 106%,with the relative standard deviations(RSDs)of 1.0%-7.9%,of which all met the detec⁃tion requirements.Furthermore,twenty-seven detergent samples bought from the market were selected for testing.The results showed that NTA and STPP were not detected in all samples,but EDTA-2Na was found in one dishwasher tablet and one baby bottle cleanser,respectively,and TSPP was detected in three dishwasher powders.GLDA was used as the chelator
作者
李晓芳
周伟
杨立威
王梦瑶
张蕾
蔡国强
LI Xiao-fang;ZHOU Wei;YANG Li-wei;WANG Meng-yao;ZHANG Lei;CAI Guo-qiang(Key Laboratory of Green Cleaning Technology&Detergent of Zhejiang Province,Lishui 323000,China;NICE Zhejiang Technology Co.Ltd.,Hangzhou 310056,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第6期699-706,共8页
Journal of Instrumental Analysis
基金
浙江省“领雁”研发攻关计划项目(2022C01174)。
关键词
离子色谱法
螯合剂
洗涤剂
同时分析
ion chromatography
chelators
detergents
simultaneous determination
