化妆品中4种禁用药物的液相色谱-串联质谱检测方法

Determination of 4 forbidden drugs in cosmetics by liquid chromatography tandem mass spectrometry

建立了水基类、乳液类和膏霜类护肤化妆品中4种氨基酸酯类禁用药物(甲丙氨酯、苯丙氨酯、己丙氨酯、环拉氨酯)的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经乙腈提取,提取液经N-丙基乙二胺(PSA)吸附剂净化后,采用液相色谱-串联三重四极杆质谱,多反应监测模式(MRM)检测,外标法定量。结果表明,甲丙氨酯、己丙氨酯和环拉氨酯在0.1~1.0 mg/kg、苯丙氨酯在0.01~0.1 mg/kg范围内线性良好,线性相关系数均大于0.997。甲丙氨酯、己丙氨酯、环拉氨酯方法检出限为0.03 mg/kg,方法定量限为0.1 mg/kg;苯丙氨酯方法检出限为0.003 mg/kg,方法定量限为0.01 mg/kg。甲丙氨酯平均回收率为88.1%~107.5%,相对标准偏差为5.4%~9.4%;苯丙氨酯平均回收率为87.6%~112.5%,相对标准偏差为4.8%~8.1%;己丙氨酯平均回收率为94.0%~109.5%,相对标准偏差为4.9%~9.4%;环拉氨酯平均回收率为91.1%~108.0%,相对标准偏差为3.7%~8.5%。方法适用于化妆品中4种禁用药物的检测。

A high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)method was developed for the determination of 4 amino-acid-ester forbidden drugs(meprobamate,phenprobamate,hexapropymate and cyclarbamate)in water based,emulsion and cream skin care cosmetics.The samples were extracted by acetonitrile,the extract solution was purified by N-(N-Propyl)ethylenediamine(PSA)sorbent,detected by HPLCMS/MS in multiple reaction monitoring mode(MRM)and quantified by external standard method.The results showed that,in the range of 0.1-1.0 mg/kg for meprobamate,hexapropymate and cyclarbamate,and in the range of0.01-0.1 mg/kg for phenprobamate,the linear correlation coefficients were all greater than 0.997.The limits of detection were 0.03 mg/kg for meprobamate,hexapropymate and cyclarbamate,and 0.003 mg/kg for phenprobamate,while the limits of quantification were 0.1 mg/kg for meprobamate,hexapropymate and cyclarbamate,and 0.01 mg/kg for phenprobamate.The average recoveries of meprobamate were 88.1%-107.5%with the relative standard deviations of 5.4%-9.4%,the average recoveries of phenprobamate were 87.6%-112.5%with the relative standard deviations of 4.8%-8.1%,the average recoveries of hexapropymate were 94.0%-109.5%with the relative standard deviations of 4.9%-9.4%,the average recoveries of cyclarbamate were 91.1%-108.0%with the relative standard deviations of 3.7%-8.5%.The method is suitable for the detection of the four forbidden drugs in cosmetics.