超高效液相色谱-质谱/质谱法同时测定蔬菜中7种磺胺的残留量

为建立超高效液相色谱-质谱/质谱法(UPLC-MS/MS)同时测定蔬菜中7种磺胺残留量的方法。样品用1%乙酸乙腈提取,以C18色谱柱分离待测物,采用多反应监测(MRM)离子扫描模式,外标法进行定量,线性良好,相关系数均大于0.999。结果显示:7种磺胺的检出限为0.000 4~0.000 6 mg/kg,样品添加回收率为67.5%~94.1%,相对标准偏差均少于5.3%(n=6)。该方法简单快捷、定量准确,可满足多种蔬菜中7种磺胺的残留检测要求。

Determination of 7 Sulfanilamide in Vegetables by UPLC-MS/MS Spectrometry

The detectable method of 7 sulfanilamide in vegetables by UPLC-MS/MS spectrometry simultaneous has been established. The samples are initially extracted with 1%acetic acid acetonitrile. The eluate is separated by gradient elution with methanol-water solution of different ratio on C18 (100 mm× 2.1 mm, 1.8 μm) column, and detected under positive multiple reactions monitoring(MRM). The external standard calibration curves are used for quantitative analysis, the correlation coefficients is higher than 0.999. The results showed that the 7 sulfanilamide detection limits is 0.000 4~0.000 6 mg/kg. The average spiked recoveries ranged from 67.5%~94.1%, and the relative standard deviations (RSDs, n=6) is less than 5.3%. The method is quick, easy and effective, it can satisfy the demand for the determination of the 7 sulfanilamide residues in vegetables.