高效液相色谱法-蒸发光散射检测器测定表面活性剂中月桂酰基甘氨酸钠含量

doi:10.3969/j.issn.1001-1803.2023.02.013

摘要/Abstract

摘要：

N-酰基氨基酸型表面活性剂是一类具有良好表活性能，且来源安全的绿色表面活性剂，被广泛用于多个领域。选取此类表面活性剂中应用较为广泛的月桂酰基甘氨酸钠（Sodium lauryl glycine，SLG）作为研究对象，为快速准确地对其进行定量分析，采用蒸发光散射检测器（ELSD）解决了该化合物紫外吸收弱而无法使用紫外检测器的问题，建立了高效液相色谱测定方法（HPLC-ELSD），并对新方法进行了方法学考察及应用。方法对提取溶剂、蒸发温度、雾化温度及载气流量等参数进行了优化，采用80%乙腈-水溶液提取样品，色谱柱为Thermo scientific Acclaim Surfactant Plus （250 mm×4.6 mm，5 μm），ELSD参数为：蒸发温度75 ℃；雾化温度85 ℃；N₂流速0.9 L/min。以乙腈-0.1 mol/L醋酸铵水溶液（乙酸调节pH值为5.4）为流动相进行梯度洗脱，测定了洗面奶中SLG的含量。结果显示：样品中SLG有较好的分离度，单次进样14 min可以完成一次完整分析。在10~200 mg/L范围内，ELSD响应值的对数与SLG质量浓度的对数线性关系良好（r=0.999 56，n=9），仪器检出限为3 mg/L，且平行样品测试的RSD<2.0%，日间精密度低于1.5%，平均加标回收率为97.4%（90.9%~100.4%）。本方法具有分析速度快，前处理简单，分离效果好，溶剂消耗少等特点，而且精密度、稳定性、回收率良好，能满足定量分析的要求，为其他N-酰基氨基酸型表面活性剂的准确测定提供了技术手段参考。

关键词: 月桂酰基甘氨酸钠, 高效液相色谱法, 蒸发光散射检测器, N-酰基氨基酸型表面活性剂

Abstract:

A method for rapid quantitative analysis of sodium lauroyl glycinate （SLG） was established by using a reversed-phase HPLC combined with evaporative light scattering detection （ELSD） without complex pre-treatment. HPLC-ELSD was equipped with Thermo Scientific Acclaim Surfactant Plus column （250 mm×4.6 mm, 5 μm）. Acetonitrile-0.1 mol/L ammonium acetate aqueous solution （the pH was adjusted to 5.4 by acetic acid） was used as the mobile phase for gradient elution and the parameters in ELSD were optimized as follows: Evaporation temperature was 75 ℃; nebulization temperature was 85 ℃; N₂flow rate was 0.9 L/min. The facial cleanser samples were extracted by mixed solvent of 80% acetonitrile-20% water and the amount of SLG was determined. The results showed that, in the range of 10-200 mg/L, the logarithm of the response value of ELSD was linearly related to the logarithm of the concentration of SLG with the correlation coefficients greater than 0.999, and the detection limit was 3 mg/L. The relative standard deviation of facial cleansing sample in 24 h was less than 1.5%, and the relative standard deviation in parallel samples was less than 2.0%. The average spike recoveries varied from 90.9% to 100.4% with standard addition. The developed HPLC-ELSD method could rapidly determine the content of SLG in facial cleansers with the advantages of simple operation, high accuracy and good reproducibility, and it was suitable for determination of other N-acylamino acid surfactants.

Key words: sodium lauroyl glycinate, HPLC, ELSD, N-acylamino acid

中图分类号:

TQ423

卓文珊, 冯顺卿, 唐建锋. 高效液相色谱法-蒸发光散射检测器测定表面活性剂中月桂酰基甘氨酸钠含量[J]. 日用化学工业（中英文）, 2023, 53(2): 220-225.

Zhuo Wenshan, Feng Shunqing, Tang Jianfeng. Determination of sodium lauroyl glycinate by HPLC-ELSD[J]. China Surfactant Detergent & Cosmetics, 2023, 53(2): 220-225.

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参考文献 14

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Time/min	0.1 mol/L Ammonium acetate aqueous solution/%	Acetonitrile/%
0.0	60	40
7.0	15	85
14.0	15	85
14.1	60	40
20.0	60	40

Extraction solvent		Area
Acetonitrile/%	Water/%	Area
80	20	3 932.8
60	40	3 922.0
40	60	3 132.1
20	80	3 179.1

Gas flow rate/ （L/min）	Area	Temperature of evaporation/℃	Area	Temperature of nebulization/℃	Area
0.9	3 527.6	75	3 499.8	85	3 527.6
1.2	2 622.3	65	3 130.1	75	3 275.7
1.5	1 488.3	55	2 547.9	65	3 164.7
1.8	892.2	45	1 181.9	55	3 107.0

Mass concentration of SLG/ （mg/L）	Area	Average area	Area RSD/%	Average RT/min	RT RSD/%
100	3 200.8	3 199.4	1.8	8.560	0.041
	3 159.4
	3 287.4
	3 211.1
	3 138.3
200	8 064.8	8 025.1	1.9	8.564	0.10
	7 769.4
	8 044.4
	8 109.6
	8 137.1

Background of SLG in facial cleanser/（mg/L）	Added/ （mg/L）	Found/ （mg/L）	Recovery/ %	Average recovery/ %	RSD/ %
43.0	10	53.8	101.4	97.4	4.0
	20	63.5	100.8
	50	92.1	99.0
	100	135.0	94.7
	150	185.3	90.9