摘要
建立了超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-QE-Orbitrap HRMS)测定动物源性食品中25种利尿剂的分析方法。畜禽肉肌肉组织经80%乙腈水溶液提取,蛋、乳样品经乙腈提取,采用PRiME HLB固相萃取柱净化后,以0.1%甲酸水溶液-乙腈为流动相在HSS T3色谱柱上进行梯度洗脱和分离,采用加热电喷雾电离源(HESI)在正负离子模式下以全扫描-数据依赖型二级扫描模式(Full MS/dd-ms^(2))进行数据采集,内标法定量。结果显示,托伐普坦、依他尼酸、阿米洛利、氨苯蝶啶、甲氯噻嗪、甲苯噻嗪均在10~200 ng/mL,其它利尿剂在5~100 ng/mL范围内线性关系良好,相关系数(r^(2))均大于0.99,检出限为5~10µg/kg,方法回收率为63.0%~116%,相对标准偏差(n=6)为0.80%~14%。该方法操作简便,实用性强,可实现动物源性食品中利尿剂类药物的快速筛查及准确定量,为动物源性食品中利尿剂的检测提供有效的技术支撑。
An analytical method was established for the determination of 25 diuretics in animal-de-rived foods by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-QE-Orbitrap HRMS).The animal meat samples were extracted with 80%acetonitrile aqueous solution,while egg and milk samples were extracted with acetonitrile.The extracts were purified through a PRiME HLB solid-phase extraction column and separated on an HSS T3 column,gradient elution with 0.1%formic acid aqueous solution and acetonitrile,simulta-neous detection by Q-Exactive Orbitrap with Full MS/dd-ms^(2) mode,under HESI positive and nega-tive ion mode.The results showed that the linearities were good in the range of 10-200 ng/mL for tolvaptan,ethacrynic acid,amiloride,triamterene,methyclothiazide and xylazine,and 5-100 ng/mL for other diuretics,with corralation coefficient(r^(2))greater than 0.99.The detection limits were in the range of 5-10µg/kg,the method recoveries were 63.0%-116%and the relative standard devia-tions(n=6)were 0.80%-14%.The method is simple and practical,and can achieve rapid screening and accurate quantification of diuretics in animal-derived foods,which could provide effective technical support for the detection of diuretics in animal-derived foods.
作者
张丽华
刘琪
李星
王羽
林立
何瑞云
姜洁
ZHANG Li-hua;LIU Qi;LI Xing;WANG Yu;LIN Li;HE Rui-yun;JIANG Jie(Beijing Institute of Food Inspection and Research(Beijing Municipal Center for Food Safety Monitoring and Risk Assessment),Key Laboratory of Key Technologies of Major Comprehensive Guarantee of Food Safety for State Market Regulation,Beijing 100094,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第10期1335-1342,共8页
Journal of Instrumental Analysis
基金
国家市场监督管理总局科技计划项目(2022MK006)。
