育发类化妆品中三种禁用物质的高效液相色谱-串联质谱测定法

Simultaneous determination of three prohibited substances in hair growth cosmetics by high performance chromatography-tandem mass spectrometry

目的建立可同时测定育发类化妆品中二苯基环丙烯酮(DPCP)、地蒽酚和维A酸含量的高效液相色谱-串联三重四级杆质谱(HPLC-MS-MS)法。方法样品用甲醇超声提取10 min,采用Luna C8色谱柱(2.0 mm×100 mm,3.0μm),以流动相为0.1%甲酸甲醇-0.1%甲酸水溶液进行梯度洗脱,流速为0.3 ml/min,柱温为25℃。采用电喷雾离子源以正离子(ESI+)多反应监测模式(MRM)进行质谱监测。结果在0.2~86.7 ng/ml的线性范围内,DPCP、地蒽酚和维A酸的回归方程均呈较好的线性关系(r>0.999)。该方法的检出限为0.3~7.4 ng/g,平均回收率:液体为90.9%~98.2%,乳液为89.6%~95.9%,凝胶为91.8%~97.2%,RSD:液体为3.7%~6.2%,乳液为3.2%~6.3%,凝胶为3.6%~6.1%。结论该方法高效、快捷、准确,适用于育发类化妆品中DPCP、地蒽酚和维A酸三种物质的同时快速检测。

Objective To establish a method for the determination of diphenylcyclopropenone(DPCP),dithranol and tretinoin in hair growth cosmetics by high performance chromatography-tandem mass spectrometry(HPLC-MS-MS).Methods The cosmetic samples were extracted by methanol under assistance of ultrasonic wave for 10 min and separated on Luna C8(2.0 mm×100 mm,3.0μm)with 0.1%(V/V)formic acid methanol and 0.1%(V/V)formic acid aqueous solution as the mobile phase for gradient elution.The flow rate was 0.3 ml/min,and the column temperature was 25℃.Multiple reaction monitoring(MRM)with positive ion mode(ESI+)was used for qualitative analysis.Results In the linear range of 0.2-86.7 ng/ml,the regression equation of three substances,including DPCP,dithranol and retinoin,showed good linear correlation(r>0.999).The limits of detection were 0.3-7.4 ng/g.The recoveries of three substances ranged 90.9%-98.2%(liquid),89.6%-95.9%(emulsion)and 91.8%-97.2%(gel)respectively,and the relative standard deviations(RSDs)ranged 3.7%-6.2%(liquid),3.2%-6.3%(emulsion)and 3.6%-6.1%(gel)respectively.Conclusion This method is accurate,sensitive,rapid and is applicable to the simultaneous determination of hair growth cosmetics.