高效液相色谱-串联质谱法测定火腿肠制品中11种杂环胺类化合物

Determination of 11 kinds of heterocyclic amines in ham sausage products by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  火腿肠制品  杂环胺类化合物

英文关键词:high performance liquid chromatography-tandem mass spectrometry  ham sausage products  heterocyclic amines

中文摘要:

      目的 建立高效液相色谱-串联质谱法同时测定火腿肠制品中11种杂环胺类化合物含量的分析方法。方法 样品经5 mL水、10 mL 1%氨水乙腈(体积分数)振荡提取后, 4 g Na2SO4, 1g NaCl盐析, 上清液经EMR-Lipid除脂小柱净化, 以HSS T3色谱柱(2.1 mm×100 mm, 1.8 μm)分离待测物, 采用电喷雾离子化, 正离子扫描和多反应监测模式检测, 以保留时间和特征离子对定性, 内标法定量。结果 11种目标化合物在2.5~40.0 μg/L范围内线性关系良好, 相关系数大于0.9950; 方法检出限为0.3~2.0 μg/kg, 定量限为1.0~ 5.0 μg/kg; 11种目标物在添加水平为5.0、10.0、20.0 μg/kg时, 平均回收率为61.7%~89.1%, 相对标准偏差为8.1%~20.4%。结论 该方法样品前处理步骤简单、耗时短, 准确性、精密度及灵敏度均较好, 适用于火腿肠制品中11种杂环胺类化合物含量的检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of the content of 11 kinds of heterocyclic amines in ham sausage products by high performance liquid chromatography-tandem mass spectrometry. Methods The sample was shaken and extracted with 5 mL water, 10 mL 1% ammonia water in acetonitrile (volume fraction), then the extraction was salted out with 4 g Na2SO4 and 1 g NaCl, the supernatant was purified by EMR-Lipid degreasing cartridge, the 11 kinds of target compounds were separated on HSS T3 column (2.1 mm×100 mm, 1.8 μm), and detected under positive ionization and multiple reaction monitoring mode. Eleven kings of compounds were identified by retention time and the ratio of characteristic ions, and the elevenheterocyclic amines were quantified by using the internal standard methods. Results The calibration curves of 11 kinds of compounds were linear within the range from 2.5 to 40.0 μg/L. The correlation coefficients of the target compounds were more than 0.9950. The limits of detection were 0.3?2.0 μg/kg, the limits of quantification were 1.0?5.0 μg/kg. The average recoveries of ham sausage samples at spiked levels (5.0, 10.0, 20.0 μg/kg) were 61.7%?89.1%, the relative standard deviations were 8.1%?20.4%. Conclusion The pretreatment of sample is simple and time-saving, the method is accurate, sensitive, which can be used to determine the content of 11 kinds of heterocyclic amines in ham sausage products.