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作 者:林庆昶 何思聪 贾晓菲 林小贞 谭淑铧 温馨 Lin Qingchang;He Sicong;Jia Xiaofei;Lin Xiaozhen;Tan Shuhua;Wen Xin(Zhongshan Quality Safety and Test Center of Agricultural Products,Zhongshan,Guangdong 528437,China)
机构地区:[1]中山市农产品质量安全检验所,广东中山528437
出 处:《绿色科技》2023年第12期179-185,共7页Journal of Green Science and Technology
摘 要:建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定禽蛋中18种磺胺类药物的方法。禽蛋样品由1%甲酸乙腈提取后,经PRiME HLB固相萃取柱净化,采用Agilent Poroshell 120 EC-C18色谱柱(100 mm×2.1 mm,2.7μm)进行分离,以0.1%甲酸水溶液和甲醇为流动相进行梯度洗脱,质谱采集采用电喷雾正离子模式,通过多反应监测(MRM)方式进行了检测。结果显示:18种磺胺类药物在1~40 ng/mL浓度范围内线性关系良好,相关系数(r 2)为0.9991~0.9999。在1.0、2.0、10.0μg/kg 3个添加水平下,其平均回收率均在70.80%~107.01%,相对标准偏差(RSD,n=6)均小于等于10.91%,方法定量限为1.0μg/kg。可见该方法准确可信、简单高效、灵敏度高,适宜应用于禽蛋中18种磺胺类药物的快速检测。A method for the determination of 18 sulfonamide residues in eggs by UPLC-MS/MS was established.The sample was extracted with acetonitrile solution containing 1%formic acid,purified by PRiME HLB solid-phase extraction column,analyzed by Agilent Poroshell 120 EC-C18 column(100mm×2.1mm,2.7μm)used 0.1%formic acid and methanol as the mobile phase,scanned by electrospray source positive ion and detected by multiple reaction monitoring mode(MRM).The results shows that there are good linear relationships between 18 sulfonamide drugs in 1-40ng/mL,with the correlation coefficient(r 2)of 0.9991~0.9999.The average recovery rates were 70.80%~107.01%and the relative standard deviation(RSD,n=6)was less than or equal to 10.91%at the three levels of 1.0,2.0 and 10.0μg/kg.The limit of quantification was 1.0μg/kg.It shows that the method is accurate,reliable,simple,rapid and high sensitivity.The method is successfully used to detect the residues of 18 sulfonamides in eggs.
关 键 词:PRiME HLB 禽蛋类食品 磺胺类药物 超高效液相色谱-串联质谱法
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