液相色谱-串联质谱法测定化妆品中丙烯酰胺单体残留量

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 (2.1 mm×150 mm,3 μm)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5~100 ng·mL^-1的范围内与丙烯酰胺(m/z 55)和内标(m/z 58)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0.01 mg·kg^-1,最低定量浓度为0.04 mg·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.