QuEChERS-超高效液相色谱-串联质谱法测定 蜂蜜中41种糖皮质激素

Determination of 41 kinds of glucocorticoids in honey by QuEChERS coupled with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  超高效液相色谱-串联质谱  糖皮质激素  蜂蜜

英文关键词:QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry  glucocorticoids  honey

中文摘要:

      目的 建立超高效液相色谱－串联质谱检测蜂蜜中41种糖皮质激素的分析方法。方法 样品用0.1%乙酸溶液及乙腈溶液提取后, 经QuEChERS分散固相萃取剂进行净化, 采用Agilent Eclipse Plus C18(100 mm× 2.1 mm, 1.8 μm)分离, 以0.1%乙酸水溶液及乙腈(含0.1%乙酸)为流动相进行梯度洗脱, 电喷雾离子源正离子多反应监测(multiple reaction monitoring, MRM)模式串联质谱进行测定。结果 在优化条件下, 41种化合物在5.0~200.0 μg/kg含量范围内有良好的线性相关性。在5.0、50、200 μg/kg添加水平的回收率为83.9%~111.2%, 相对标准偏差(relative standard deviation, RSD, n=6)小于10%。结论 该方法快速、简单、准确, 适用于蜂蜜中41种糖皮质激素残留的定性、定量分析。

英文摘要:

      Objective To establish a method for the determination of 41 kinds of glucocorticoids in honey by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS /MS). Methods The samples were extracted with 0.1% acetic acid solution and acetonitrile, and were purified by QuEChERS disperse solid phase extraction agent. The separation was performed on a Agilent Eclipse Plus C18(100 mm×2.1 mm, 1.8 μm) with gradient elution using 0.1% acetic acid solution and acetonitrile (containing 0.1% acetic acid). The analytes were determined by electrospray ion source and multiple reaction monitoring (MRM) mode with mass spectrometry. Results With the optimal conditions, 41 kinds of glucocorticoids had good linear relationships in the range of 5.0-200.0 μg/kg. The recoveries of 3 different spiked levels (5.0, 50, 200 μg/kg) were 83.9%-111.2%, with the relative standard deviations of less than 10%. Conclusions This method is rapid, simple and credible, which is suitable for the qualitative and quantitative analysis of 41 kinds of glucocorticoids residues in honey.