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    高效液相色谱-串联质谱法测定化妆品中非法添加的米诺地尔

    HPLC-MS/MS Determination of Minoxidil of Illegal Addition in Cosmetics

    • 摘要: 采用高效液相色谱-串联质谱法测定化妆品中非法添加的米诺地尔的含量。样品以饱和氯化钠溶液盐析破乳,用乙腈超声提取20 min,离心后,取上清液过0.22 μm滤膜。以ACQUITY UPLC® BEH C18色谱柱为固定相,以不同体积比的0.2%(体积分数,下同)乙酸溶液和0.2%乙酸甲醇溶液的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾正离子源和多反应监测模式,采用同位素内标法定量。米诺地尔的线性范围为5~500 μg·L-1,检出限(3S/N)为1 ng·g-1。以空白样品为基体进行加标回收试验,所得回收率为108%~114%,回收量的相对标准偏差(n=6)为1.2%~2.8%。

       

      Abstract: HPLC-MS/MS was applied to the determination of minoxidil of illegal addition in cosmetics. Saturated sodium chloride solution was added in the sample for salting out and demulsification. The sample solution was extracted ultrasonically for 20 min with acetonitrile. After centrifugation, the supernatant was filtered on 0.22 μm filtering membrane. ACQUITY UPLC® BEH C18 chromatographic column was used as stationary phase, and the mixture of 0.2% (φ, the same below) acetic acid solution and 0.2% acetic acid methanol solution mixed in different ratios was used as mobile phase in gradient elution. ESI+ and multi-reactions monitor mode were adopted in MS/MS. Isotope was used as internal standard. Linearity range of minoxidil were found in the range of 5-500 μg·L-1 with detection limit (3S/N) of 1 ng·g-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 108%-114%, with RSDs (n=6) of recovery amounts in the range of 1.2%-2.8%.

       

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