化妆品中托萘酯、利拉萘酯的高效液相色谱定量及 高效液相色谱-串联质谱确证

Determination of tolnaftate and liranaftate in cosmetics by high performance liquid chromatography and verification by high performance liquid chromatography-tandem mass spectrometry

建立了化妆品中托萘酯、利拉萘酯的高效液相色谱法(HPLC)和高效液相色谱-串联质谱(HPLC-MS/MS)确证方法。以乙腈为提取溶剂,经涡旋、超声制成样品溶液。在HPLC方法中,采用5μm粒径的常规C18色谱柱,以乙腈和0.1%甲酸水为流动相,在258和283 nm波长下进行定量测定,同时结合200~400 nm范围光谱进行定性。HPLC-MS/MS方法所用流动相与HPLC法相同,经粒径为1.8μm的高效C18柱分离,用ESI源在MRM模式下对目标物进行确证。在HPLC方法中,托萘酯和利拉萘酯的线性范围分别为0.1~10.0 mg/L和0.2~20.0 mg/L(R^(2)>0.99),检出限为3.0和6.0 mg/kg,定量限为10和20 mg/kg,加标回收率为93.3%~107.9%(RSD<5%)。在HPLC-MS/MS方法中,托萘酯和利拉萘酯的线性范围均为0.05~5.00μg/L(R^(2)>0.99),检出限均为0.002 mg/kg,定量限均为0.005 mg/kg,加标回收率为84.0%~112.8%(RSD<5%)。本研究建立的方法简便、快速、专属性强、准确度高,适用于化妆品中托萘酯和利拉萘酯的测定。

A method for the determination of tolnaftate and liranaftate in cosmetics by high performance liquid chromatography(HPLC)and verification by high performance liquid chromatography-tandem mass spectrometry(HPLCMS/MS)was established.Samples(including 5 kinds of matrix:cream,emulsion,liquid,gel,and oil)were extracted with acetonitrile,mixed thoroughly by vortex and ultra-sonication.In HPLC method,the separation was performed by C18 column of 5μm particle sizes using acetonitrile and 0.1%formic acid water as mobile phases at the wavelength of 258 nm and 283 nm.The HPLC-MS/MS method employed a rapid resolution C18 column of 1.8μm particle sizes and the same mobile phases as the HPLC method.The target compounds were analyzed by multiple reaction monitoring(MRM)in electro-spray ionization(ESI)mode.Both the HPLC and HPLC-MS/MS methods show good performance in methodology validation.In HPLC method,the linearities of tolnaftate and liranaftate are in the range of 0.1-10.0 mg/L and 0.2-20.0 mg/L,respectively(correlation coefficient,R^(2)>0.99),the limits of detection(LOD)are 3.0 mg/kg and 6.0 mg/kg,the limits of quantitation(LOQ)are 10 mg/kg and 20 mg/kg,and the spiked recoveries are between 93.3%and 107.9%(relative standard deviation,RSD<5%).While in HPLC-MS/MS method,the linearities of tolnaftate and liranaftate both are 0.05-5.00μg/L(R^(2)>0.99),the LODs are 0.002 mg/kg,the LOQs are 0.005 mg/kg,and the spiked recoveries are between 84.0%and 112.8%(RSD<5%).The method established in this study is simple,rapid,with strong specificity and high accuracy and is suitable for the determination of tolnaftate and liranaftate in cosmetics.