摘要
建立了超高效液相色谱-串联质谱(UPLC-MS/MS)检测化妆品还原液中4-氨基联苯的方法。化妆品试样经过连二亚硫酸钠化学还原后,离心、PCX固相萃取小柱提取富集、净化,并经氨化甲醇洗脱、氮吹至近干,定容后通过UPLC-MS/MS仪检测,分离柱为Waters Acquity BEH C18柱;流动相为0.3%乙腈-甲酸水溶液;流速0.5mL/min。5种不同基质中4-氨基联苯在5~250ng/mL浓度范围内呈良好的线性关系,线性回归系数r2均大于0.999,检测限均为1ng/mL。5种不同基质中4-氨基联苯的回收率为80.9%~92.6%,相对标准偏差(RSD)为0.51%~3.76%(n=3)。
A simple and rapid method was developed for the determination of 4-aminodiphenyl reduced from azo dyes in cosmetics by ultra performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method. After chemically reduced with sodium dithionite, the cosmetic sample was centrifuged, extracted, purified by PCX solid-phase extraction column, eluted with ammonia methanol and dried under nitrogen. After the chromatographic separation on Waters Acquity BEH C18 column(100 × 2.1 mm, 1. 7um) by 0. 3% formicacid-acetonitrileisocratic elution, the analysis was carried out by UPLC-MS/MS. The linear ranges of 4-aminobiphenyl in five cosmetic matrices were 5-250 ng/mL(r2 〉 0. 999) and the detection limits were 1 ng/mL. The recoveries were ranged from 80. 9% to 92. 6%, and the relative standard deviations were 0.51%-3.76 % (n= 3).
出处
《分析科学学报》
CAS
CSCD
北大核心
2012年第6期831-834,共4页
Journal of Analytical Science
基金
福建省自然科学基金(No.2010J05019)
福建省卫生厅基金(2010-1-34)