固相萃取-高效液相色谱/质谱联用-测定祛痘类化妆品中8种非法添加的药物

Determination of 8 illegal added drugs in anti-acne cosmetics by SPE- HPLC-MS/MS

关键词:  液相色谱/质谱联用  非法添加药物  固相萃取  祛痘类化妆品

Key words:  HPLC-MS/MS  illegal addition of drugs  solid phase extraction  anti-acne cosmetics

摘要:

目的 采用固相萃取-高效液相色谱-串联质谱(SPE-HPLC-MS/MS)法建立同时测定3 种不同基质类型(水剂、乳液类和膏霜类)祛痘化妆品中氟康唑、酮康唑、硝酸益康唑、硝酸咪康唑、盐酸萘替芬、他扎罗汀、依曲替酯、维胺酯等8种化妆品中非法添加药物的检测方法。 方法 化妆品样品经含有1%的四氢呋喃的甲醇溶液提取后,采用HLB 固相萃取柱净化后上机检测,经ZORBAX-C₁₈分离,0.1%甲酸水溶液-含0.1%甲酸的甲醇溶液作为流动相梯度洗脱,在电喷雾离子源(ESI)正离子模式下电离,多反应监测(MRM)模式下测定,基质匹配标准曲线外标法定量。结果 8种化合物在各自浓度范围内线性关系良好,相关系数均不低于0.995,检出限为0.075-2.8 mg.kg_-1^,定量限为0.22-5.4mg.kg_-1^,平均回收率为89.5 % -103.1 %,RSD 均<10%。结论 本法简单准确,灵敏度高,可用于市售祛痘类化妆品中8种非法添加药物的检测。

Abstract:

To establish a High performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method for simultaneous separation and determination of eight illegal added drugs in anti-acne cosmetics which contained fluconazole, naftifine hydrochloride, ketoconazole, econazole, miconazole nitrate, tazarotene, etretinate and viaminate (water aqua, lotion and cream) by solid phase extraction. METHODS Samples were ultrasonically extracted by methanol solution (containing 1% tetrahydrofuran), then purified by HLB solid phase extraction column. Samples were separated by ZORBAX-C18 column. The mobile phase consisted of 0.1% formic acid aqueous solution-methanol aqueous solution (including 0.1% formic acid) by gradient elution, electrospray ionization source was applied and operated in the positive mode. Multiple reaction monitoring mode was used to monitor ions. Matrix matching calibration method was used for the quantification. RESULTS The results showed that the eight compounds had good linear relationship in their respective concentration range, the correlation coefficient was not less than 0.995, the detection limit was 0.075-2.8 mg·kg??, the quantitative limit was 0.22-5.4mg·kg-1, and the average recovery was 89.5 %-103.1 %, RSD was less than 10%. CONCLUSION The method is simple, accurate and sensitive, which can be used for the detection of eight illegal added drugs in anti-acne cosmetics.