UPLC-Q-TOF-MS法同时测定椰油酰胺丙基甜菜碱中一氯乙酸、二氯乙酸和羟基乙酸

doi:10.3969/j.issn.1001-1803.2019.10.011

日用化学工业 ›› 2019, Vol. 49 ›› Issue (10): 694-698.doi: 10.3969/j.issn.1001-1803.2019.10.011

• 分析与检测 • 上一篇

UPLC-Q-TOF-MS法同时测定椰油酰胺丙基甜菜碱中一氯乙酸、二氯乙酸和羟基乙酸

黄芳,王玉芹,邓欣,谢淑桐,黄晓兰,吴惠勤

中国广州分析测试中心广东省分析测试技术公共实验室,广东广州 510070

收稿日期:2019-03-05 修回日期:2019-09-22 出版日期:2019-10-22 发布日期:2019-10-24
通讯作者: 吴惠勤
作者简介:黄芳（1975-）,女,硕士,高级工程师,主要从事有机质谱分析与应用,电话：13642741616,邮箱： 13642741616@139.com。
基金资助:
广东省食品药品监督管理局科技创新项目资助(2018TDZ18)

Simultaneously determination of monochloroacetic acid, dichloroacetic acid and glycollic acid in cocamidopropyl betaine by UPLC-Q-TOF-MS

HUANG Fang,WANG Yu-qin,DENG Xin,XIE Shu-tong,HUANG Xiao-lan,WU Hui-qin

Guangdong Provincial Public Laboratory of Analysis and Testing Technology, China National Analytical Center（Guangzhou）, Guangzhou, Guangdong 510070, China

Received:2019-03-05 Revised:2019-09-22 Online:2019-10-22 Published:2019-10-24
Contact: Hui-qin WU

摘要/Abstract

摘要：

建立了液相色谱-四极杆飞行时间质谱同时测定椰油酰胺丙基甜菜碱表面活性剂中一氯乙酸、二氯乙酸和羟基乙酸的方法。样品经水溶解后固相萃取小柱净化,经核壳型亚3 μm填料色谱柱Agilent Poroshell 120 EC-C₁₈（3.0 mm× 100 mm×2.7 μm）分离,以0.1%（V/V）甲酸和乙腈为流动相梯度洗脱,采用电喷雾离子源负离子全扫描模式采集后,提取精确离子定性定量。经方法验证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0.997,3个添加水平的平均回收率在71.1%~92.2%之间,相对标准偏差（RSD）小于15%,方法检出限分别为：一氯乙酸0.25 mg/kg,二氯乙酸0.025 mg/kg,羟基乙酸10 mg/kg。

关键词: 液相色谱-四极杆飞行时间质谱, 椰油酰胺丙基甜菜碱, 一氯乙酸, 二氯乙酸, 羟基乙酸

Abstract:

A method based on ultra-high performance liquid chromatography with quadrupole time-of-flight mass spectrometry（UPLC-Q-TOF-MS） had been developed for the simultaneous determination of monochloroacetic acid, dichloroacetic acid and glycollic acid in cocamidopropyl betaine surfactant. The samples were dissolved by water, then purified by solid phase extraction and separated by a core-shell sub-3 μm column Agilent Poroshell 120 EC-C₁₈（3.0 mm×100 mm×2.7 μm） with a gradient elution of 0.1% formic acid and acetonitrile. Under electrospray ion source negative ion full scan mode, the extracted accurate ion was used to do qualitative and quantitative determination. The results show that the linearity of the three compounds is good in a certain concentration range, and the correlation coefficients are greater than 0.998.The average recovery of the three levels ranges from 71.1% to 92.2%, and the relative standard deviation（RSD） is less than 15%. The detection limits of the optimized method are 0.25 mg/kg for monochloroacetic acid, 0.025 mg/kg for dichloroacetic acid and10 mg/kg for glycollic acid.

Key words: UPLC-Q-TOF-MS, cocamidopropyl betain, monochloroacetic acid, dichloroacetic acid, glycollic acid

中图分类号:

TQ423

黄芳,王玉芹,邓欣,谢淑桐,黄晓兰,吴惠勤. UPLC-Q-TOF-MS法同时测定椰油酰胺丙基甜菜碱中一氯乙酸、二氯乙酸和羟基乙酸[J]. 日用化学工业, 2019, 49(10): 694-698.

HUANG Fang,WANG Yu-qin,DENG Xin,XIE Shu-tong,HUANG Xiao-lan,WU Hui-qin. 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.

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参考文献 14

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保留时间/min	名称	分子式	CAS号	理论定量离子 [M-H]^-的m/z	实测定量离子 [M-H]^-的m/z	质量准确度误差
2.71	一氯乙酸	C₂H₃ClO₂	79-11-8	92.974 9	92.974 7	<1×10^-6
2.40	二氯乙酸	C₂H₂Cl₂O₂	79-43-6	126.935 9	126.935 9	<1×10^-6
1.66	羟基乙酸	C₂H₄O₃	79-14-1	75.008 8	75.008 6	<1×10^-6

序号	成分名称	线性方程	线性范围/（mg·L^-1）	相关系数（r）	检出限/（mg·kg^-1）	定量限/（mg·kg^-1）
1	一氯乙酸	Y=17 461X-1 332	0.1~500	0.999 1	0.25	1.0
2	二氯乙酸	Y=76 909X-5 328	0.01~500	0.997 7	0.025	0.1
3	羟基乙酸	Y=1 966.7X-107.3	1.0~200	0.998 6	10	20

成分名称	添加量/（mg·kg^-1）	回收率/%	RSD/%
一氯乙酸	1.0	76.8	13.3
	10.0	82.6	9.8
	50.0	88.2	9.7
二氯乙酸	0.1	78.1	12.2
	1.0	84.5	9.2
	10.0	81.8	6.1
羟基乙酸	50	71.1	14.2
	100	89.7	9.7
	200	92.2	7.9

序号	一氯乙酸含量/ （mg·kg^-1）	二氯乙酸含量/ （mg·kg^-1）	羟基乙酸含量/%
1	未检出	103	0.27
2	未检出	188	0.10
3	未检出	43.0	0.32
4	3.5	79.3	0.091
5	1.4	0.10	0.064
6	未检出	未检出	0.19
7	未检出	未检出	0.10
8	未检出	4.4	0.14
9	未检出	22.8	0.22
10	未检出	19.3	0.17
11	未检出	0.15	0.11
12	6.6	177	0.12
13	127	384	0.23
14	49.1	251	0.18

UPLC-Q-TOF-MS法同时测定椰油酰胺丙基甜菜碱中一氯乙酸、二氯乙酸和羟基乙酸

Simultaneously determination of monochloroacetic acid, dichloroacetic acid and glycollic acid in cocamidopropyl betaine by UPLC-Q-TOF-MS

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