高效液相色谱-三重四极杆质谱法测定化妆品中的西咪替丁及雷尼替丁

doi:10.3969/j.issn.1001-1803.2020.09.011

摘要/Abstract

摘要：

建立可同时测定化妆品中西咪替丁及雷尼替丁的高效液相色谱-三重四极杆质谱方法。待测样品经甲醇超声提取,经0.2 μm滤膜过滤后进样检测,在优化的色谱、质谱条件下,经ZORBAX SB-Aq色谱柱分离。采用电喷雾离子源在正离子模式下进行多反应监测。用基质匹配外标曲线法进行定量分析。结果表明,西咪替丁、雷尼替丁的检出浓度分别为0.03和0.02 ng/g,在1~100 ng/mL范围内线性关系良好（r >0.999）,低、中、高3个质量浓度水平下的样品加标回收率为84.9%~116.2%,RSD不超过5%。建立的方法前处理过程简单,灵敏度、线性、回收率及重复性均满足方法学要求,可同时对化妆品中的西咪替丁和雷尼替丁进行测定。

关键词: 化妆品, 西咪替丁, 雷尼替丁, 抗组胺, 高效液相色谱-三重四极杆质谱法

Abstract:

A high performance liquid chromatography-tandem mass spectrometric method was established for determination of cimetidine and ranitidine in cosmetics. Samples were extracted by methanol ultrasonically, and then filtered through a 0.2 μm membrane. After separated by a ZORBAX SB-Aq column, samples were detected by MRM with electrospray ion source in positive mode. Matrix-matched external standard calibration curves were used for quantitative analysis. The concentration limits of detection of cimetidine and ranitidine were 0.03 and 0.02 ng/g, respectively. In the mass concentration range of 1-100 ng/mL, cimetidine and ranitidine showed good linear relationship with correlation coefficients all above 0.999．The recoveries for cimetidine and ranitidine at three spiked levels were in the range of 84.9%-116.2%, and the relative standard deviations of their recoveries were not more than 5%. This method was able to be applied in determination of cimetidine and ranitidine in cosmetics with simple pretreatment, good linearity and high recovery.

Key words: cosmetics, cimetidine, ranitidine, antihistamine, high performance liquid chromatography-tandem mass spectrometric method

中图分类号:

TQ658

王聪,李莉,王海燕,孙磊. 高效液相色谱-三重四极杆质谱法测定化妆品中的西咪替丁及雷尼替丁[J]. 日用化学工业, 2020, 50(9): 643-647.

WANG Cong,LI Li,WANG Hai-yan,SUN Lei. Determination of cimetidine and ranitidine in cosmetics by high performance liquid chromatography-tandem mass spectrometry[J]. China Surfactant Detergent & Cosmetics, 2020, 50(9): 643-647.

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参考文献 16

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时间/min	φ（A）/%	φ（B）/%
0	95	5
6	10	90
9	10	90
9.1	95	5
12	95	5

化合物	保留时间/min	母离子	定量离子	定性离子	碰撞能量/V
西咪替丁	3.3	253.1	117.0	117.0;159.2	32;42
雷尼替丁	3.4	315.1	176.1	176.1;130.1	28;42

化合物	基质	回归方程	相关系数	线性范围/(ng·mL^-1)	基质效应/%
西咪替丁	无	y=377x-629	0.999 6	1.13~113
	液态水基	y=214x+59	0.999 8	1.13~113	-43.2
	膏霜	y=282x-187	0.999 8	1.13~113	-25.2
	乳液	y=313x+212	0.999 8	1.13~113	-17.0
雷尼替丁	无	y=575x+306	0.999 9	0.990~99.0
	液态水基	y=229x+28	0.999 8	0.990~99.0	-60.2
	膏霜	y=439x+68	0.999 9	0.990~99.0	-23.7
	乳液	y=461x+908	0.999 6	0.990~99.0	-19.8

化合物	基质	回收率/%			回收率RSD/%			重复性RSD/%
化合物	基质	低浓度	中浓度	高浓度	低浓度	中浓度	高浓度	重复性RSD/%
西咪替丁	乳液	98.0~103.6	89.8~93.5	99.0~100.4	3.0	2.0	0.8	3.5
	膏霜	107.6~116.2	85.8~90.8	96.2~99.1	4.0	2.9	0.9	1.4
	液态水基	99.0~100.4	89.5~91.0	95.2~96.2	0.9	1.7	0.5	3.9
雷尼替丁	乳液	84.9~90.8	100.3~113.5	109.3~113.7	3.4	1.6	2.1	2.3
	膏霜	101.5~105.7	106.8~115.9	106.5~110.6	2.0	4.1	1.9	1.0
	液态水基	97.8~108.1	104.1~108.3	104.5~107.6	5.0	2.2	1.6	6.9