高效液相色谱-三重四极杆串联质谱法同时测定化妆品中24种香豆素类化合物

Determination of 24 coumarin compounds in cosmetics by high performance liquid chromatography-tandem mass spectrometry

建立了高效液相色谱-三重四级杆串联质谱法同时测定化妆品中24种香豆素类化合物含量。水基、乳液、膏霜类样品和唇膏、粉饼等固态类样品分别采用甲醇、甲醇-四氢呋喃(1∶1)混合溶液超声提取后,经Agilent Poroshell 120 SB-C18色谱柱(100 mm×4.6mm,2.7μm)分离,以甲醇-5 mmol/mL甲酸铵(含0.1%甲酸)溶液作为流动相进行梯度洗脱,流量为0.5 mL/min,多反应监测模式检测。24种香豆素类化合物在各自质量浓度范围内与色谱峰面积线性关系良好,相关系数均不小于0.9995,检出限为0.002~0.8μg/kg,定量限为0.004~3μg/kg。在低、中、高三个浓度加标水平下,样品平均加标回收率为84.8%~112.9%,测定结果的相对标准偏差为1.2%~9.8%(n=6)。该方法操作简便、灵敏度高、准确性好,可用于化妆品中香豆素类化合物的定性筛查和定量测定。

A method based on high performance liquid chromatography-tandem mass spectrometry was established for determining 24 coumarin compounds in cosmetics.Methanol,methanol-tetrahydrofuran(1/1)were used for water�based,emulsion,cream samples and solid samples such as lipstick and powder,respectively.Compounds were separated on an Agilent Poroshell 120 SB-C18(4.6 mm×100 mm,2.7μm)column,and gradient elution was carried out with methanol-5 mmol/L ammonium formate solution(containing 0.2% formic acid)as the mobile phase.The flow rate was 0.5 mL/min.Multi reaction monitoring was used.24 coumarin compounds showed good linearity with the correlation coefficient not less than 0.9995 in their respective mass concentrations.The limits of detection and limits of quantification were 0.002-0.8μg/kg and 0.004-3μg/kg,respectively.Under the three spiked levels of low,medium and high,the average recoveries ranged from 84.8% to 112.9%,and the relative standard deviations were between 1.2% and 9.8%(n=6).This method is simple,fast,sensitive,accurate and suitable for the determination of 24 coumarins in cosmetics.