QuEChERS-高效液相色谱-串联质谱法快速测定牛奶中18 种糖皮质激素类药物残留  

Rapid Determination of 18 Glucocorticoids in Milk Using QuEChERS Coupled with Liquid ChromatographyTandem Mass Spectrometry

作　　者：田海伟 冯浩彬 李晋[1] 李丽丽[1] 李挥[2] 哈婧[1] TIAN Haiwei;FENG Haobin;LI Jin;LI Lili;LI Hui;HA Jing(College of Chemical and Pharmaceutical Engineering, Hebei University of Science and Technology, Shijiazhuang 050018, China;Hebei Food Safety Key Laboratory, Shijiazhuang 050200, China)

机构地区：[1]河北科技大学化学与制药工程学院,河北石家庄050018 [2]河北省食品安全重点实验室,河北石家庄050200

出　　处：《食品科学》2017年第12期310-314,共5页Food Science

基　　金：河北省科技计划项目(15275505D);北京市重点实验室开放课题(BKBD-2016KF(01))

摘　　要：通过Qu ECh ERS前处理方法,结合高效液相色谱-串联质谱多反应监测模式下的定性和定量分析,实现牛奶中18种糖皮质激素的同时检测。牛奶样品加入酸化乙腈溶剂提取后,加入氯化钠和无水硫酸镁进行盐析,经PSA、C_(18)吸附剂净化后,取上清液进行高效液相色谱-串联质谱分析。方法的基质效应影响在0.81~0.96之间,方法检出限在0.1~0.3μg/kg之间,定量限在0.3~1.1μg/kg之间,在0.5~100 ng/m L范围内呈线性关系,目标物线性相关系数(R^2)均大于0.993 6,3个水平加标回收率在73.7%~98.6%之间,精密度(n=5)在4.9%~12.9%之间。该方法简单快捷、准确可靠,适合于大批量牛奶样品中糖皮质激素的快速检测。A simple,rapid and sensitive method for the simultaneous determination of18kinds of glucocorticoids in milkwas developed by the quick,easy,cheap,effective,rugged and safe(QuEChERS)method coupled with high performanceliquid chromatography-tandem mass spectrometry(HPLC-MS/MS)in the multiple reaction monitoring(MRM)mode.Milksamples were extracted with acidified acetonitrile,and salted out by adding sodium chloride anhydrous sodium magnesiumsulfate.After purification with PSA and C18as the adsorbent,the supernatant was analyzed by HPLC-MS/MS.The matrixeffect in the method was in the range of0.81–0.96,the limits of detection(LODs)were in the range of0.1–0.3μg/kg andthe limits of quantification(LOQs)for the analytes were in range of0.3–1.1μg/kg.The method exhibited a good linearrelationship in the range of0.5–100ng/mL,with a correlation coefficient(R2)of higher than0.9936,and recoveries werebetween73.7%and98.6%at three spiked levels with relative standard deviations(n=5)of4.9%–12.9%.This method wassimple,accurate,reliable,and suitable for the rapid detection of glucocorticoids in bulk serum samples.

关 键 词：牛奶 QUECHERS 糖皮质激素 高效液相色谱-串联质谱 

分 类 号：O656[理学—分析化学]