QuEChERS-高效液相色谱-三重四极杆质谱法检测乳及乳制品中2-己基吡啶含量

Determination of 2-hexylpyridine content in milk and dairy product by QuEChERS-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  2-己基吡啶  乳及乳制品  液相色谱-串联质谱法

英文关键词:2-hexylpyridine  milk and dairy product  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-三重四极杆质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定乳及乳制品中2-己基吡啶含量的分析方法。方法 样品经乙腈涡旋提取, 分析液经QuEChERS dSPE EMR-Lipid除脂专用管净化, 离心后过膜上机检测。测试方法以乙腈-一级水为流动相, 流速设置为0.25 mL/min, 应用梯度洗脱程序, 采用GL Sciences InertSustain C18色谱柱进行分离, 电喷雾正离子(electro spray ionization, ESI+)模式, 多反应监测(multiple reaction monitoring, MRM)模式检测, 基质匹配外标法进行定量。结果 对于乳及乳制品基质, 2-己基吡啶在0.5~20.0 ng/mL的质量浓度与其相对应的峰面积之间线性关系良好, 相关系数(r2)均大于0.998, 在0.005、0.010和0.050 mg/kg 3种不同浓度添加水平下, 2-己基吡啶的平均回收率为94.45%~109.63%, 相对标准偏差为3.93%~9.53%。结论 本方法可满足乳及乳制品中2-己基吡啶检测的正确度、精密度和灵敏度的要求。

英文摘要:

      Objective To establish a method for the determination of 2-hexylpyridine content in the milk and dairy product by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The sample was extracted by acetonitrile vortex extraction, and the analytical solution was purified by QuEChERS dSPE EMR Lipid degreasing tube. After centrifugation, it was tested on a membrane machine. The acetonitrile primary water as the mobile phase was used, the flow rate was set at 0.25 mL/min, the gradient elution procedure was applied, the GL Sciences InertSustain C18 chromatographic column was used for separation, the electro spray positive ion (ESI+) mode, the multiple reaction monitoring (MRM) mode was used for detection, and the matrix matching external standard method was used for quantification. Results The methodological validation indicators were well that the calibration curves were linear in the range of 0.5–20.0 ng/mL with the correlation coefficients (r2) larger than 0.998. The average recoveries of 2-hexylpyridine were 94.45%–109.63% and the relative standard deviations were 3.93%–9.53% at 0.005, 0.010 and 0.050 mg/kg with 3 kinds of spiked levels. Conclusion The accuracy, precision, and sensitivity of the method meet the requirements for residue detection.