液相色谱-串联质谱法测定乳制品中盐酸普萘洛尔残留量

Determination of propranolol hydrochloride in dairy products by liquid chromatography-tandem mass spectrometry

中文关键词:  液相色谱-质谱联用仪  盐酸普萘洛尔  乳制品

英文关键词:liquid chromatography-tandem mass spectrometry  propranolol hydrochloride  dairy products

中文摘要:

      目的 建立了乳制品中盐酸普萘洛尔残留的液相色谱-串联质谱检测方法(liquid chromatography- tandem mass spectrometry, LC-MS/MS)。方法 乳制品用乙腈提取, 提取液用甲酸酸化后, 经正己烷去除油脂以及N-丙基乙二胺净化, 微孔滤膜过滤后进样。C8柱分离后采用多反应监测(multiple reaction monitoring, MRM)模式进行检测, 外标法定量。结果 目标化合物在1.56~25.0 μg/L范围内线性关系良好, 相关系数(r2)大于0.999。固体乳制品中盐酸普萘洛尔的定量限(limit of quantitation, LOQ)和检出限(limit of detection, LOD)分别为2.00 μg/kg、1.00 μg/kg; 液体乳制品中盐酸普萘洛尔的定量限(LOQ)和检出限(LOD)分别为0.40 μg/L、0.20 μg/L; 不同加标浓度样品(LOQ、2LOQ、10LOQ)的平均回收率为93.4%~108%, 相对标准偏差(relative standard deviations, RSDs)为2.90%~5.80%。35份市售乳制品中均未检出盐酸普萘洛尔残留。结论 该方法简便、快速、准确, 精密度、检出限等参数均能满足相关的技术规范的要求, 可用于市售乳制品的检测。

英文摘要:

      Objective To establish a method for determination of propranolol hydrochloride in dairy products by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Dairy products were extracted with acetonitrile, the extract was acidified with formic acid and the oil was removed with n-hexane, and the sample was purified with n-propyl ethylenediamine, and filtered by microporous membrane. After C8 column separation, the analyte was determined by LC-MS/MS in multiple reaction monitoring (MRM) and quantified by external standard method. Results The target compound had a good linear relationship within the range of 1.56-25.0 μg/L, and the correlation coefficient (r2) was greater than 0.999. The limit of quantification (LOQ) and limit of detection (LOD) of the solid dairy products were 2.00 μg/kg and 1.00 μg/kg, respectively. The LOQ and LOD of the liquid dairy products were 0.40 μg/L and 0.20 μg/L, respectively. The average recoveries varied from 93.4% to 108% (n=6) with the relative standard deviations (RSDs) of 2.90%-5.80% at 3 spiked levels (LOQ, 2LOQ and 10LOQ). No traces of propranolol hydrochloride were found in 35 commercially sold dairy products. Conclusion This method is simple, rapid and accurate, and the precise, limit of detection and other parameters of the method can meet the requirements of relevant technical specifications, which can be used for the detection of commercially available dairy products.