液相色谱-串联质谱法测定火腿肠和咸菜中亚硝酸盐含量

Determination of nitrite in ham sausage and pickles by liquid chromatography-tandem mass spectrometry

中文关键词:  亚硝酸盐  火腿肠  咸菜  液相色谱-串联质谱法

英文关键词:nitrite  ham sausage  pickle  liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立一种亚硝酸盐检测的液相色谱-串联质谱检测方法, 并用于火腿肠和咸菜中亚硝酸盐的测定。方法 样品经硼砂溶液提取, 亚铁氰化钾和乙酸锌沉淀蛋白后, 使用对氨基苯磺酸和盐酸萘乙二胺进行 衍生化。采用0.1%甲酸(A)和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱, 质谱采用多离子检测模式(multi-reaction monitoring, MRM)对衍生化产物的定量离子和定性离子进行监测定量。结果 本方法在2~ 200 μg/L浓度范围内线性良好。方法重复性相对标准偏差(relative standard deviation, RSD) <5%(n=6), 在1、5和10 mg/kg添加水平的回收率为85.0%~101.3%, 定量限为0.12 mg/kg。结果不受提取液本底颜色的影响。 结论 该方法快速、准确、灵敏, 测得样品火腿肠和咸菜中亚硝酸盐含量为5.20~52.51 mg/kg。

英文摘要:

      Objective To establish a method for determination of nitrite by liquid chromatography-tandem mass spectrometric (LC-MS/MS), and detect nitrite in ham sausage and pickle samples. Methods After the samples were extracted with borax solution, protein was precipitated with potassium ferrocyanide and zinc acetate, and samples were derived with p-aminobenzene sulfonic acid and naphthylenediamine hydrochloride. The 0.1% formic acid (A) and 0.1% formic acid-acetonitrile (B) were used as mobile phases for gradient elution. Quantitative and qualitative ions of the derivative products were monitored and quantified by mass spectrometry using multi-reaction monitoring (MRM). Results The method has a good linearity in the range of 2-200 μg/L, with the repeatability relative standard deviation (RSD) less than 5% (n=6). The recovery rates were 85.0%-101.3% at spiked levels of 1, 5 and 10 mg/kg. The limit of quantitative was less than 0.12 mg/kg. Detection was not affected by the color of the substrate. Conclusion This method is rapid, accurate and sensitive, and the nitrite content of ham sausage and pickles samples are 5.20-52.51 mg/kg