QuEChERS/超高效液相色谱-串联质谱法同时测定防晒化妆品中15种香豆素与10种二苯甲酮类化合物

Simultaneous Determination of 15 Coumarins and 10 Benzophe⁃nones in Sunscreen Cosmetics by QuEChERS/Ultra-high Perfor⁃mance Liquid Chromatography-Tandem Mass Spectrometry

建立了防晒化妆品中15种香豆素与10种二苯甲酮类化合物的QuEChERS/超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。防晒霜、粉底、隔离、喷雾等不同类型的化妆品样品采用乙腈提取,50 mg C18与150 mg无水MgSO4吸附剂净化。采用Zorbax SB-C_(18)(RRHD)色谱柱(2.1 mm×150 mm,1.8μm)分离,0.1%甲酸水溶液(含5 mmol/L乙酸铵)和乙腈为流动相梯度洗脱,电喷雾离子源正离子模式、多反应监测扫描模式进行测定,外标法定量,粉底和喷雾样品以基质匹配标准溶液外标法定量。结果显示,25种待测组分在各自质量浓度范围内线性关系良好,相关系数(r)均不低于0.995。对于防晒霜和隔离类样品,方法检出限(LOD)为0.005~0.450μg/g,定量下限(LOQ)为0.010~0.750μg/g;对于粉底与喷雾类样品,方法检出限为0.005~0.500μg/g,定量下限为0.010~1.000μg/g。25种待测组分的平均回收率为80.8%~113%,相对标准偏差为0.20%~6.8%。样品溶液中25种待测组分在48 h内稳定。该方法前处理简单、灵敏、准确,适用于化妆品中香豆素与二苯甲酮类化合物的同时检测。

A QuEChERS/ultra-high performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS)method was established for the simultaneous determination of 15 coumarins and 10 benzophenones in sunscreen cosmetics.The samples including cream,foundation,isolation and spray were extracted with acetonitrile,and purified with a combined adsorbent of 50 mg C18 and 150 mg anhydrous MgSO4.The chromatographic separation for the analytes was achieved on a Zorbax SB-C18(RRHD)column(2.1 mm×150 mm,1.8μm).Gradient elution was performed using 0.1%formic acid solution(containing 5 mmol/L ammonium acetate)and acetonitrile.Then the analytes were de⁃termined with electrospray ionization in positive ion mode under multiple reaction monitoring(MRM),and quantified by external standard method,while the analytes in foundation and spray samples were quantified by matrix-matched external standard method.The experimental results indicated that good linearities were observed for 25 kinds of analytes in the respective concentration ranges,with their correlation coefficients(r)larger than 0.995.The limits of detection(LODs)and limits of quantita⁃tion(LOQs)for cream and isolation samples were in the ranges of 0.005-0.450μg/g and 0.010-0.750μg/g,while the LODs and LOQs for foundation and spray samples were 0.005-0.500μg/g and 0.010-1.000μg/g,respectively.Mean recoveries for the analytes at three spiked levels ranged from 80.8%to 113%,with relative standard deviations(RSDs)of 0.20%-6.8%.Moreover,the analytes in the sample solutions were stable within 48 hours.The proposed method is simple,sensitive and accurate,and it could be applied to the simultaneous determination of coumarin and benzophenone compounds in cosmetics.