采用超高效液相色谱-大气压化学电离源-三重四极杆串联质谱法测定化妆品中的丙烯酰胺残留。以水为萃取溶剂萃取样品中的丙烯酰胺,萃取液经C18固相萃取柱净化后,在Waters Atlantic T3色谱柱上分离,以0.1%(φ)甲酸溶液-甲醇为洗脱液进行梯度洗脱。质谱分析中采用大气压化学电离源和多反应监测模式。丙烯酰胺的质量浓度在1.0~20.0 μg·L-1范围内与峰面积呈线性关系,检出限(3S/N)为0.001 mg·kg-1,测定下限(10S/N)为0.01 mg·kg-1。加标回收率在90.8%~108%之间,测定值的相对标准偏差(n=6)小于7.0%。采用该方法分析15批次不同的化妆品,有一批次样品检出丙烯酰胺,质量分数为1.2 mg·kg-1。

UHPLC-MS/MS with atmospheric pressure chemical ionization (APCI) and triple quadrupole was applied to the determination of acrylamide residue in cosmetics. Water was used as the solvent to extract acrylamide from the sample, and the extracted solution was purified with a C18 solid phase extraction column and then separated on a Waters Atlantic T3 chromatographic column with a mixture of 0.1% (φ) formic acid and methanol as the mobile phase for gradient elution. APCI and MRM were adopted in MS analysis. Linear relationship was found between the peak area and the mass concentration of acrylamide in the range of 1.0-20.0 μg·L-1, with detection limit (3S/N) of 0.001 mg·kg-1 and the lower limit of determination (10S/N) of 0.01 mg·kg-1. Recovery obtained by standard addition method were in the range of 90.8%-108% and RSD′s (n=6) were less than 7.0%. The method was used to analyze 15 different batches of cosmetics and acrylamide was detected in one sample with the mass fraction of 1.2 mg·kg-1.