CAJ | 학술논문

以C18和MCX串联固相萃取柱作为净化手段，建立检测豆制品、米线和年糕中违禁添加物乌洛托品含量高效液相色谱-串联质谱法（HPLC-MS/MS）的方法。在电喷雾正离子模式下，采用选择反应监测模式（SRM），用目标物的保留时间和质谱碎片丰度比来定性，外标法定量。结果表明：乌洛托品在0.5～100.0μg/L浓度范围线性良好，相关系数为0.9994，方法的检出限为0.25μg/kg，定量限为2.5μg/kg，阴性样本添加水平为5、10、20μg/kg时，平均回收率为85.1％～105.1％，相对标准偏差（RSD）为0.9%～4.4％。该方法具有准确、快速、简单以及灵敏度高的特点，能够适应大规模样品的快速分析要求。
이C18화MCX천련고상췌취주작위정화수단，건립검측두제품、미선화년고중위금첨가물오락탁품함량고효액상색보-천련질보법（HPLC-MS/MS）적방법。재전분무정리자모식하，채용선택반응감측모식（SRM），용목표물적보류시간화질보쇄편봉도비래정성，외표법정량。결과표명：오락탁품재0.5～100.0μg/L농도범위선성량호，상관계수위0.9994，방법적검출한위0.25μg/kg，정량한위2.5μg/kg，음성양본첨가수평위5、10、20μg/kg시，평균회수솔위85.1％～105.1％，상대표준편차（RSD）위0.9%～4.4％。해방법구유준학、쾌속、간단이급령민도고적특점，능구괄응대규모양품적쾌속분석요구。
A method of liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed to monitor methenamine which illegally added in soy products,rice flour,rice pastry and purified by C18 and MCX cartridges. The target compound was detected by Selective Reaction Monitoring(SRM) atelectro spray positive ionization (ESI+) mode, external standard method was adopted to quantify. The results indicated that methenamine can reach a good linear relationship within the concentration range of 0.5 to 100.0μg/L with R2=0.9994, the method of limits of detection (LOD) and the method of limits of quantitation (LOQ) were respectively 0.25μg/kg and 2.5μg/kg. At the spiking levels of 5、10、20μg/kg,the average recoveries in foods ranged 85.1% from 105.1%, RSDs ranged 0.9% from 4.4%. This proposed method was rapid, accuracy, strong specificity, high sensitivity. Methenamine was easy to operate and satisfied with fast speed. The conclusion in this study might showed it is suitable for the quantitative determination methenamine in soy products rice flour and rice pastry.