摘要
目的:建立HPLC-MS/MS法测定化妆品中丙烯酰胺单体残留量。方法:以Atlantis C18色谱柱(2.1mm×150mm,3μm)为固定相,以0.1%甲酸溶液-0.1%甲酸甲醇溶液(98:2)为流动相A,0.1%甲酸甲醇溶液为流动相B进行梯度洗脱。以同位素13C3-丙烯酰胺为内标,样品用0.1%甲酸溶液提取后,以石油醚液液萃取后进样,以保留时间及质谱图定性,以MRM方式监测,测定丙烯酰胺单体残留量。结果:丙烯酰胺浓度在5～100ng.mL-1的范围内与丙烯酰胺(m/z55)和内标(m/z58)峰面积的比值呈良好线性关系(r=0.9995,n=6)。高、中、低3种浓度的平均回收率均在80.5%～102.5%之间,RSD为1.8%～7.2%。最低检出浓度为0.01mg.kg-1,最低定量浓度为0.04mg.kg-1。结论:方法灵敏度高、重现性好,适用于各种化妆品中丙烯酰胺单体残留量的测定。
Objective：To establish a liquid chromatography coupled with electrospray ionization tandem mass spectrometry （LC-MS/MS） method for the identification and quantification of acrylamide residues in cosmetic products.Method：After addition of internal standard of 13 C3-acrylamide,extraction with 0.1% formic acid in water,defatting with petroleum ether,the test solution was injected into an Atlantis C18 column （2.1 mm×50 mm,3 μm） using 0.1% formic acid in water-0.1% formic acid in methanol （98：2） as mobile phase A,0.1% formic acid in methanol as mobile phase B in a gradient elution mode.A positive electrospray ionization and multiply reaction monitoring （MRM） was employed.Results：The linear range of acrylamide was 5-100 ng·mL-1 （r=0.9995,n=6）,and the average spiked recoveries were between 80.5%-102.5% with RSD of 1.8%-7.2%.The limit of detection （LOD） was 0.01 mg·kg-1,and the limit of quantitation was 0.04 mg·kg-1.Conclusion：The proposed method has been successfully applied for the determination of acrylamide residues in cosmetics with satisfactory results for its sensitivity,precision and repeatability.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2010年第10期1887-1890,共4页
Chinese Journal of Pharmaceutical Analysis
基金
上海市食品药品监督管理局课题(No.B2009J2-017)
