高效液相色谱法测定醇醚羧酸盐中羟基乙酸、一氯乙酸和二氯乙酸的含量

doi:10.3969/j.issn.1001-1803.2022.10.015

摘要/Abstract

摘要：

建立了一种高效液相色谱法测定醇醚羧酸盐产品中羟基乙酸、一氯乙酸和二氯乙酸含量的方法。样品经流动相溶解后直接进样分析,采用具有反相和阴离子交换两种分离模式的Acclaim Trinity P1色谱柱（3.0 mm×150 mm,3 μm）进行分离,以体积分数为10%乙腈-90%磷酸缓冲盐水溶液（10 mmol磷酸二氢钠,调节pH为5.0）洗脱,在紫外检测器210 nm波长下检测。经方法学验证,3种化合物在一定质量浓度范围内线性良好,相关系数均大于0.999,测定精密度、稳定性皆满足要求,测定平均回收率在96%~98%之间,相对标准偏差（RSD）皆小于3%。与GB/T 28193–2011《表面活性剂中氯乙酸（盐）残留量的测定》方法相比,该方法测定结果接近,但增加了羟基乙酸的测定,结果更加全面。与离子色谱法相比,该方法不受产品溶解性限制,可用于高碳链或水溶性不佳的产品体系,适用范围更宽。

关键词: 醇醚羧酸盐, 羟基乙酸, 一氯乙酸, 二氯乙酸, 高效液相色谱

Abstract:

A method for determination of glycolic acid, monochloroacetic acid and dichloroacetic acid in alkylpolyethoxy carboxylate （AEC） by high performance liquid chromatography was established. The column was Acclaim Trinity P1 column （3.0 mm×150 mm, 3 μm） for separation and it was adapted gradient with 10% acetonitrile-90% phosphate buffered saline （10 mmol sodium dihydrogen phosphate, adjust pH to 5.0）. A UV detector at 210 nm was used. The separation and determination of glycolic acid, monochloroacetic acid and dichloroacetic acid could be completed. The resolution of chromatographic peaks of the three compounds to be tested in the sample solution is good, and the peak area and concentration of the reference substance show good linear correlation, and the correlation coefficients are greater than 0.999. The stability and precision of the analysis meet the requirements of methodological investigation. The average recovery of three compounds is in the range from 96% to 98%, and the relative standard deviation （RSD） is less than 3%. Compared with the method of GB/T 28193—2011 （Determination of chloroacetic acid （chloroacetate） contents in surfactants）, this method is not limited by product solubility, and can be used in product systems with long carbon chain or poor water solubility. Therefore, it has a wider scope of application, and it can provide references for AEC product quality control, production process upgrading and test method improvement.

Key words: alkylpolyethoxy carboxylate, glycolic acid, monochloroacetic acid, dichloroacetic acid, high performance liquid chromatography

中图分类号:

TQ423

张军,杨秀全,周媛,白亮,吴志宇. 高效液相色谱法测定醇醚羧酸盐中羟基乙酸、一氯乙酸和二氯乙酸的含量[J]. 日用化学工业（中英文）, 2022, 52(10): 1135-1139.

Zhang Jun,Yang Xiuquan,Zhou Yuan,Bai Liang,Wu Zhiyu. Determination of glycolic acid, monochloroacetic acid and dichloroacetic acid in alkylpolyethoxy carboxylate by HPLC[J]. China Surfactant Detergent & Cosmetics, 2022, 52(10): 1135-1139.

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参考文献 6

[1]	Lu Xuejun, Tao Huadong, Zhang Yiyong. Research progress in alcohol ether carboxylate surfactant[J]. Detergent & Cosmetics, 2014, 37 (11): 21-23.
[2]	Han Jianying, Feng Yu. Research on the improvement of QB/T 2950—2008: determination of monochloroacetic acid (salt) in AEC surfactant products[J]. Detergent & Cosmetics, 2016, 39 (6): 17-22.
[3]	Standardization Administration of the P.R.C. Determination of chloroacetic acid (chloroacetate) contents in surfactants: GB/T 28193—2011[S]. 2011.
[4]	Cui Shiyong, Jiang Lihua. Determination of monochloroacetic acid and dichloroacetic acid in surfactants by ion chromatography[J]. Chin. J. Health Lab. Tec., 2013, 23 (18): 3486-3488.
[5]	Liu Zhenhua, Zhang Yong. Determination of GCA, MCA and DCA in betaine and carboxylate surfactants by ion chromatography[J]. China Cleaning Industry, 2014 (8): 45-48.
[6]	Huang Fang, Wang Yuqin, Deng Xin. Simultaneously determination of monochloroacetic acid, dichloroacetic acid and glycollic acid in cocamidopropyl betaine by UPLC-Q-TOF-MS[J]. China Surfactant Detergent & Cosmetics, 2019, 49 (10): 694-698.

羟基乙酸含量/%	RSD/%	一氯乙酸含量/‰	RSD/%	二氯乙酸含量/‰	RSD/%
1.07	1.15	0.026 1	1.88	0.026 3	1.81
1.10		0.025 2		0.025 5
1.08		0.025 0		0.025 2

序号	羟基乙酸含量/mg	加标量/mg	测得量/mg	回收率/%	平均回收率/%	RSD/%
1	27.5	27.5	54.1	96.7	97.9	0.72
2	27.4	27.5	54.3	97.8
3	27.2	27.5	54.0	97.5
4	27.6	27.5	54.8	98.9
5	27.8	27.5	54.9	98.5
6	27.3	27.5	54.2	97.8

序号	一氯乙酸含量/μg	加标量/μg	测得量/μg	回收率/%	平均回收率/%	RSD/%
1	62.5	62.5	123.5	97.6	97.0	0.75
2	62.3	62.5	123.1	97.3
3	62.4	62.5	122.5	96.2
4	62.1	62.5	123.2	97.8
5	62.2	62.5	122.1	95.8
6	62.4	62.5	123.1	97.1

序号	二氯乙酸含量/μg	加标量/μg	测得量/μg	回收率/%	平均回收率/%	RSD/%
1	170.0	170.0	336.3	97.8	96.8	1.28
2	166.6	170.0	334.2	98.6
3	167.8	170.0	333.1	97.2
4	171.1	170.0	332.5	94.9
5	172.2	170.0	336.7	96.8
6	169.9	170.0	332.6	95.7

方法	羟基乙酸含量/%	均值/%	一氯乙酸含量/‰	均值/‰	二氯乙酸含量/‰	均值/‰
本文方法	1.07	1.08	0.026 1	0.025 4	0.069 1	0.069 5
	1.10		0.025 2		0.068 3
	1.08		0.025 0		0.071 0
GB/T 28193—2011方法	未规定	/	0.023 1	0.024 2	0.071 2	0.071 5
			0.025 3		0.073 0
			0.024 2		0.070 4