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超高效液相色谱-串联质谱法测定化妆品中36种兴奋剂

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利用超高效液相色谱-串联质谱仪(UPLC-MS/MS),建立了一种同时测定化妆品中蛋白同化制剂、β2激动剂、糖皮质激素、刺激剂、大麻酚类等36种兴奋剂的检测方法.化妆品样品经甲醇超声提取后,以0.1%乙酸水溶液和甲醇-乙腈混合溶液(体积比1∶9)作为流动相,使用Waters ACQUITY UPLC BEH C18色谱柱(3.0mm×150mm,1.7μm)进行梯度分离.目标物在电喷雾正负离子模式下,以多反应监测(MRM)方式进行测定,用外标法定量.结果表明,在1.0~20ng/mL的质量浓度范围内,36种兴奋剂组分的线性关系良好(r>0.995),检出限为1.0~3.0μg/kg,定量限为3.3~9.9μg/kg.3种基质样品在低、中、高3个加标水平下的平均回收率为80.6%~115.3%,相对标准偏差为0.5%~12.9%(n=5).该方法前处理操作简便,快速,灵敏度高,结果准确,适用于常见化妆品中多类兴奋剂组分的快速检测.
Determination of 36 stimulants in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry
An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS)method was developed for the simultaneous determination of 36 stimulants including anabolic agents,β2 agonists,glucocorticoids,irritants,and cannabinoids in cosmetics.In this study,pretreatment operation and instruments parameters were also optimized.Cosmetic samples were ultrasonically extracted by methanol,and then the separation of 36 stimulants was carried out on a Waters ACQUITY UPLC BEH C18 column(3.0 mm×150 mm,1.7 μm)by gradient elution,using 0.1%acetic acid solution and methanol-acetonitrile(1∶9,by volume)as the mobile phase.The 36 target compounds were analyzed in positive and negative electrospray ionization mode under multiple reaction monitoring(MRM)mode.Meanwhile,the analytes were quantified by external standard method,and the linear regression analysis data show that there are good linear relationships for 36 target compounds in the mass concentration range of 1.0-20 ng/mL,with their correlation coefficients(r)greater than 0.995.The limits of detection(LOD)and limits of quantitation(LOQ)of the method are in the ranges of 1.0-3.0 μg/kg and 3.3-9.9 μg/kg,respectively.The recoveries for 36 target compounds in three kinds of matrix samples at three spiked levels are between 80.6%and 115.3%,with the relative standard deviations(RSD)of 0.5%-12.9%(n=5).The method is simple,rapid,high sensitivity,accurate and suitable for the rapid detection of many stimulants in cosmetics.

ultra performance liquid chromatography-tandem mass spectrometrystimulantcosmetics

徐炜、邹坡、李长于、杨铭、鹿燕、李慧良

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杭州宜格化妆品有限公司,浙江 杭州 310000

浙江方圆检测集团股份有限公司,浙江 杭州 310000

超高效液相色谱-串联质谱法 兴奋剂 化妆品

浙江省市场监督管理局雏鹰计划培育项目

CY2022005

2024

日用化学工业(中英文)
中国日用化学工业研究院

日用化学工业(中英文)

CSTPCD北大核心
影响因子:0.553
ISSN:1001-1803
年,卷(期):2024.54(3)
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