高效液相色谱-串联质谱法测定婴幼儿化妆品中微量丙烯酰胺

Determination of acrylamide residue in baby cosmetics by HPLC-MS/MS

建立液液萃取法-HPLC-MS/MS法测定不同化妆品基质中丙烯酰胺的残留量。以ACEEXCEL3C18-AR(100×4.6 mm,3μm)为固定相,以乙腈-0.1%甲酸水为流动相,等度洗脱,样品采用二氯甲烷-0.1%甲酸水溶液进行液液萃取,取上清液进行HPLC-MS/MS测定,ESI正离子扫描,MRM监测,以保留时间及相对丰度比定性,内标法测定丙烯酰胺的残留量。结果表明,在三类不同基质的化妆品中丙烯酰胺质量浓度在2.5~2 500μg/L范围内均具有良好的线性关系,相关系数(r)均大于0.995,不同质量浓度水平下的回收率为86.9%~113.5%,精密度为0.6%~10.4%,定量限均为0.025 mg/kg,油状和乳状基质中检出限为0.005 mg/kg,膏霜类基质中为0.008 mg/kg。该方法准确可靠,适用于不同基质化妆品中丙烯酰胺残留量的测定。

To establish a liquid-liquid extraction HPLC-MS/MS method for the identification and quantification of acrylamide in three cosmetics matrixes. The cosmetics were dissolved in dichloromethane and the acrylamide was extracted with 0.1% formic acid. The extracted solution was separated on an ACE EXCEL 3 C18-AR(100×4.6 mm, 3 μm) chromatographic column with a mixture of 0.1% formic acid and acetonitrile as mobile phase for isocratic elution and detected with a triple quadrupole mass analyzer using ESI with positive ionization. Ions was monitored in the multiple reaction mode. The acrylamide was identified with relative retention time and ion abundance ratio, and quantified by internal standard method. The established method showed a good linearity in the mass concentration range of 2.5-2 500 μg/L with a LOQ of 0.025 mg/kg for acrylamide in three kinds of cosmetics matrix. The LOD of oil and emulsion matrix were 0.005 mg/kg, and the LOD of cream-like matrix was 0.008 mg/kg. The extraction recovery and precision were 86.9%-113.5% and 0.6%-10.4%, respectively. The established liquid-liquid extraction HPLC-MS/MS method is proved to be accurate and sensitive, and can be applied to determine acrylamide in different cosmetic products.