采用高效液相色谱-串联质谱法测定膏霜类消毒产品中丙酸氯倍他索和盐酸左氧氟沙星的含量。样品用乙腈提取20 min,所得萃取液以Thermo Hypersil Gold色谱柱为分离柱,以不同体积比的0.1%(φ)甲酸溶液和乙腈混合液为流动相进行梯度洗脱,采用电喷雾正离子源多反应监测模式检测。2种化合物的质量浓度均在0.50~100 μg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.06~0.009 μg·kg-1之间。在0.50,5.0,50.0 μg·L-1等3个浓度水平进行加标回收试验,回收率在90.0%~95.6%之间,测定值的相对标准偏差(n=5)在1.9%~4.0%之间。

HPLC-MS/MS was applied to the determination of clobetasol propionate and levofloxacin hydrochloride in cream disinfection products. The sample was extracted with acetonitrile for 20 min. The extract obtained was separated by using Thermo Hypersil Gold chromatographic column as stationary phase, and mixtures of 0.1% (φ) formic acid solution and acetonitrile (mixed in various ratios) as mobile phase in gradient elution. ESI+ and multi-reactions monitoring were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 2 compounds were kept in the same range of 0.50-100 μg·L-1, with detection limits (3S/N) in the range of 0.06-0.009 μg·kg-1. Tests for recovery were made by standard addition method at the concentration levels of 0.50, 5.0, 50.0 μg·L-1, giving values of recovery in the range of 90.0%-95.6%, and values of RSD′s (n=5) found were in the range of 1.9%-4.0%.