A method of liquid chromatography-tandem mass spectrometry(LC-MS/MS) was developed to monitor methenamine which illegally added in foods.Anhydrous sodium sulfate was used for drying and dehydration,and the solution of acetonitrile was used for extracting methenamine.Then,a strong cation exchange(SCX) was applied to separate target compound with gradient elute.The target compound was detected by Multiple Reaction Monitoring(MRM) at electro spray positive ionization(ESI+) mode.The external standard method was adopted to quantify.The calibration curves showed good linearity for target compound with the detection range of 1～ 1000μg/L.Correlative coefficient was 0.998 8,the method of limits of detection(LOD) and the method of limits of quantitation(LOQ) were respectively 0.2 μg/kg and 1.0 μg/kg,respectively.The spiked recoveries in foods ranged 52.6％ from 118％ with RSDs less than 10.2％.This proposed method was rapid,accuracy,strong specificity,high sensitivity.Pretreatment was easy to operate and satisfied with fast speed.The conclusion in this study showed it is suitable for the quantitative determination methenamine in foods.%建立测定乌洛托品的高效液相色谱-串联质谱法,用于快速监测食品中违法添加的乌洛托品.食品中乌洛托品经无水硫酸钠干燥脱水,乙腈提取后,采用梯度洗脱,SCX色谱柱分离,在电喷雾正离子模式下,多反应监测模式进行检测,外标法定量.乌洛托品在1～1 000 μg/L浓度范围线性良好,相关系数为0.998 8,方法的检出限为0.2 μg/kg,定量限为1.0 μg/kg,加标回收率在52.6％～118％,相对标准偏差小于10.2％.本方法快速、准确,特异性强,灵敏度高,样品前处理简便易行,分析周期短,适合大量样品的测定.
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