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[目的]建立一种超高效液相色谱-串联质谱测定茶叶中氯噻啉残留量的方法。[方法]样品用乙腈匀质提取,经GC-e/NH2柱去除杂质,经C18液相柱分离后,用电喷雾离子化-串联质谱测定。[结果]在12.5~100.0滋g/L质量浓度范围内,氯噻啉工作曲线相关系数(R2)为0.994 5,仪器最小检出量为5.98×10-13 g。在0.025、0.25、2.50 mg/kg添加水平下,茶叶中氯噻啉回收率在94.66%~96.30%之间,相对标准偏差小于8.0%,方法最低检出限为0.99×10-3mg/kg。采用该方法对实际样品进行测定,均未检出氯噻啉残留。[结论]方法准确、快速、稳定,能够满足实际残留检测的需要。
[Objective] To establish a method for the determination of chlorothiazine residues in tea by ultra performance liquid chromatography-tandem mass spectrometry. [Method] The samples were homogenized with acetonitrile, separated by GC-e / NH2 column, separated by C18 liquid column and determined by electrospray ionization-tandem mass spectrometry. [Result] The correlation coefficient (R2) of chlorothiazine working curve was 0.994 5 in the range of 12.5-100.0 μg / L, and the minimum detectable amount was 5.98 × 10-13 g. Under the condition of 0.025,0.25 and 2.50 mg / kg, the recovery of chlorothiazide in tea was between 94.66% and 96.30%, the relative standard deviation was less than 8.0%. The detection limit was 0.99 × 10-3mg / kg. The method was used to determine the actual samples, but no chlorothiazine residue was detected. [Conclusion] The method is accurate, rapid and stable, which can meet the need of actual residual testing.