CAJ | 학술논문

目的：建立腐竹中乌洛托品的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法。方法样品经乙腈/水(1：1,v：v)溶液超声提取,阳离子交换柱净化后,经Waters Acquity UPLC BEH HILIC(2.1 mm ×100 mm,1.7μm)色谱柱分离,在电喷雾正离子多反应监测模式下进行测定。结果乌洛托品在0.5~100.0μg/L范围内线性关系良好,相关系数(r)大于0.999。方法检出限和定量限分别为6μg/kg和20μg/kg。在20、40、100μg/kg 3个空白加标水平下,乌洛托品的加标回收率为100.1%~103.9%,相对标准偏差为4.7%~8.9%。结论该方法快速、简便、准确可靠,适用于腐竹中非法添加的乌洛托品的含量测定。
목적：건립부죽중오락탁품적초고효액상색보-천련질보(UPLC-MS/MS)측정방법。방법양품경을정/수(1：1,v：v)용액초성제취,양리자교환주정화후,경Waters Acquity UPLC BEH HILIC(2.1 mm ×100 mm,1.7μm)색보주분리,재전분무정리자다반응감측모식하진행측정。결과오락탁품재0.5~100.0μg/L범위내선성관계량호,상관계수(r)대우0.999。방법검출한화정량한분별위6μg/kg화20μg/kg。재20、40、100μg/kg 3개공백가표수평하,오락탁품적가표회수솔위100.1%~103.9%,상대표준편차위4.7%~8.9%。결론해방법쾌속、간편、준학가고,괄용우부죽중비법첨가적오락탁품적함량측정。
Objective To establish a method for the determination of urotropine in dried beancurd sticks by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).MethodsSamples were ultrasonically extracted by acetonitrile/water (1:1,v:v), and then purified by cation exchange solid phase extraction. The analytes were separated on a Waters Acquity UPLC BEH HILIC column (2.1 mm × 100 mm, 1.7μm) and detected by positive electrospray ionization in multiple reactions monitoring (MRM).Results The method showed a good linearity over the range of0.5~100.0μg/L with relative coefficient not less than 0.999. The limit of detection (LOD) and the limit of quantification (LOQ) were 6μg/kg and 20μg/kg, respec-tively. The average recoveries of urotropine at the spiking levels of 20, 40 and 100μg/kg were in the range of 100.1%~103.9%, with the relative standard deviations in the range of 4.7%~8.9%.ConclusionThe method is rapid, simple and accurate for the determination of urotropine in dried beancurd sticks.