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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
引用本文:田海伟,冯浩彬,李晋,李丽丽,李挥,哈婧.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[J].食品科学,2017,38(12):310-314.
作者姓名:田海伟  冯浩彬  李晋  李丽丽  李挥  哈婧
作者单位: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
基金项目: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。

关 键 词:牛奶  QuEChERS  糖皮质激素  高效液相色谱-串联质谱  

Rapid Determination of 18 Glucocorticoids in Milk Using QuEChERS Coupled with Liquid Chromatography-Tandem Mass Spectrometry
TIAN Haiwei,FENG Haobin,LI Jin,LI Lili,LI Hui,HA Jing.Rapid Determination of 18 Glucocorticoids in Milk Using QuEChERS Coupled with Liquid Chromatography-Tandem Mass Spectrometry[J].Food Science,2017,38(12):310-314.
Authors:TIAN Haiwei  FENG Haobin  LI Jin  LI Lili  LI Hui  HA Jing
Affiliation:1. College of Chemical and Pharmaceutical Engineering, Hebei University of Science and Technology, Shijiazhuang 050018, China; 2. Hebei Food Safety Key Laboratory, Shijiazhuang 050200, China
Abstract:A simple, rapid and sensitive method for the simultaneous determination of 18 kinds of glucocorticoids in milk was developed by the quick, easy, cheap, effective, rugged and safe (QuEChERS) method coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) in the multiple reaction monitoring (MRM) mode. Milk samples were extracted with acidified acetonitrile, and salted out by adding sodium chloride anhydrous sodium magnesium sulfate. After purification with PSA and C18 as the adsorbent, the supernatant was analyzed by HPLC-MS/MS. The matrix effect in the method was in the range of 0.81–0.96, the limits of detection (LODs) were in the range of 0.1–0.3 μg/kg and the limits of quantification (LOQs) for the analytes were in range of 0.3–1.1 μg/kg. The method exhibited a good linear relationship in the range of 0.5–100 ng/mL, with a correlation coefficient (R2) of higher than 0.993 6, and recoveries were between 73.7% and 98.6% at three spiked levels with relative standard deviations (n = 5) of 4.9%–12.9%. This method was simple, accurate, reliable, and suitable for the rapid detection of glucocorticoids in bulk serum samples.
Keywords:milk  QuEChERS  glucocorticoids  high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)  
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