超高效液相色谱-串联质谱法测定凉茶中10种硝基咪唑类物质

Determination of 10 kinds of nitroimidazole substances in herbal tea by ultra performance liquid chromatography-tandem mass spectrometry

目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定凉茶中硝基咪唑类物质含量的方法。方法 试样经50%甲醇水溶液超声提取,采用T_(3)色谱柱(2.1 mm×100 mm,1.6μm)分离,建立UPLC-MS/MS测定二甲硝咪唑、羟基二甲硝咪唑、异丙硝唑、羟基甲硝唑、羟基异丙硝唑、氯甲硝咪唑、洛硝哒唑、替硝唑、奥硝唑、甲硝唑10种成分含量的方法。结果 UPLC-MS/MS检测10种成分平均回收率为64.9%~118.0%,精密度为2.0%~13.0%,在一定浓度范围内,线性关系均大于0.99,检出限为0.025~0.125 mg/kg,定量限为0.050~0.250 mg/kg。结论 该方法操作简单、准确性高、稳定性好,可用于凉茶中10种硝基咪唑类成分的定量分析。

Objective To establish a method for the determination of nitroimidazole compounds in herbal tea by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The sample was extracted by ultrasound with 50% methanol aqueous solution and separated using a T_3(2.1 mm × 100 mm,1.6 μm)chromatographic column.A method was established for the determination of the content of 10 kinds of components,including dimetridazole,1-methyl-5-nitro-2-hydroxymethylimidazole,ipronidazole,metronidazole-OH,Ipronidazole-hydroxy,5-chloro-1-methyl-4-nitroimid-azole,ronidazole,tindazole,ornidazole,and metronidazole,using UPLC-MS/MS.Results The average recovery rates of 10 kinds of components detected by UPLC-MS/MS ranged from 64.9%-118.0%,with precision ranging from 2.0%-13.0%.Within a certain concentration range,the linear relationship was greater than 0.99.The detection limit was 0.025–0.125 mg/kg,and the limits of quantification were 0.050–0.500 mg/kg.Conclusion This method is easy to operate,has high accuracy,and good stability,and can be used for quantitative analysis of 10 kinds of nitroimidazole components in herbal tea.