QuEChERS-超高效液相色谱-串联质谱法快速测定化妆品中糖皮质激素类药物

Rapid determination of glucocorticoids in cosmetics by QuEChERS-ultra performance liquid chromatography tandem mass spectrometry

目的建立QuEChERS-超高效液相色谱-串联质谱法快速测定化妆品中16种糖皮质激素类药物的检测方法。方法样品经1%(V/V)甲酸-乙腈提取,加入氯化钠进行盐析,提取液经C_(18)50 mg、N-丙基乙二胺(primary secondary amine,PSA)100 mg、MgSO_(4)150 mg净化,采用Thermo Acclaim RSLC 120 C_(18)(2.1 mm×100 mm,2.2μm)进行分离,电喷雾正离子多反应监测扫描(multiple reaction monitoring,MRM)模式下进行测定,外标法定量。结果16种糖皮质激素在线性范围1~100 ng/mL内线性良好,相关系数r^(2)在0.991~0.999之间,方法定量限为10μg/kg,16种糖皮质激素平均回收率在76.5%~109.3%之间,相对标准偏差为0.77%~2.41%。结论该方法操作简单、净化效果好、灵敏度、准确度和精密度均符合多残留检测技术要求,解决了化妆品中糖皮质激素类药物检测提取过程过于繁琐的问题,可为化妆品检测提供更方便、更快捷的检测方法支持。

Objective To establish a method for the rapid determination of 16 glucocorticoids in cosmetics by QuEChERS-ultra performance liquid chromatography tandem mass spectrometry.Methods Samples were extracted by 1%(V/V)formic acid and acetonitrile and added with NaCl for salting out.The extract was purified by C_(18)50 mg,primary secondary amine(PSA)100 mg and MgSO_(4)150 mg,and Thermo Acclaim RSLC 120 C_(18)(2.1 mm×100 mm,2.2μm)was used for separation.Electrospray positive ion multiple reaction monitoring(MRM)mode was used to determine the content and the external standard method was used for quantitative analysis.Results The linear range of 16 glucocorticoids was 1-100 ng/mL,and the correlation coefficient r^(2)was 0.991-0.999.The recovery rates of 16 glucocorticoids were between 76.5%and 109.3%,the relative standard deviations(RSDs)was 0.77%-2.41%.Conclusion This method is simple,effective,sensitive,accurate and precise,and meets the requirements of multi-residue detection technology.It solves the problem that the detection and extraction process of glucocorticoids in cosmetics is too complicated,which can provide more convenient and faster detection method support for cosmetics detection.