超高效液相色谱-串联质谱法测定化妆品中的腈菌唑

Determination of myclobutanil in cosmetics by liquid chromatography-tandem mass spectrometry

建立了超高效液相色谱-串联质谱法测定化妆品中腈菌唑的方法。试样经乙腈提取,正己烷萃取除去脂溶性杂质,氮气吹干富集,采用 UPLC-MS/MS,以 C18色谱柱分离,电喷雾电离（ESI）,正离子,多反应监测（ MRM）模式检测,外标法定量。在1～100 ng·mL-1范围内,线性相关系数0．99；添加回收率范围82．4～91．5%,相对标准偏差（RSD）4．8%～9．5%,方法定量下限0．5μg·kg-1。该方法快速、检测灵敏度高,可适用于各类化妆品中腈菌唑的测定。

A method for determination of myclobutanil in cosmetics by ultra performance liquid chromatography-tandem mass spec-trometric was established. The samples were extracted with acetonitrile,and then hexane was used to remove the fat-soluble impuri-ties. The purified samples were enriched with nitrogen gas and were injected into UPLC-MS/MS. The analysis was carried out in the multiple reaction monitoring（ MRM） mode by employing the external standard method. The calibration curves showed good linearity in the range of 1 ～100 ng·ml-1 with correlation coefficients larger than 0. 99. The average recoveries were between 82. 4% ～91. 5%with RSD of 4. 8% ～9. 5%. The limit of quantitation（LOQ）was 0. 5μg·kg-1. The method is fast-speed,high sensitivity,and could be applied for quantitative determination of myclobutanil residue in cosmetics.