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| 超高效液相色谱-串联质谱法测定食品中一种新型非法添加物伐地那非杂质31 |
| Determination of a new illegal additive, vardenafil impurity 31 by ultra performance liquid chromatography-tandem mass spectrometry |
| 投稿时间：2024-09-11 修订日期：2025-05-10 |
| DOI： |
| 中文关键词: 超高效液相色谱-串联质谱法 高分辨质谱 非法添加物 |
| 英文关键词:UPLC-MS/MS HRMS Illegal additives |
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| 中文摘要: |
| 目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定食品中一种新型非法添加物伐地那非杂质31的定性定量检测方法。方法 运用UPLC-MS/MS对待测试样中92种那非类非法添加物质进行筛查，运用超高效液相色谱-高分辨质谱法(ultra performance liquid chromatography-high resolution mass spectrometry, UPLC-HRMS)对待测试样进行结构解析，推断出结构后，购入标准品经验证后，确认待测试样中目标物为伐地那非杂质31，采用UPLC-MS/MS建立多反应监测(multiple reaction monitoring, MRM)方法，定性定量测定食品中伐地那非杂质31。结果 本方法伐地那非杂质31的检出限为5 μg/kg，定量限为10 μg/kg。在0.1~50.0 ng/mL的线性范围内线性关系良好，相关系数(r)为0.9976，平均加标回收率在85.33%~89.41%之间，相对标准偏差(relative standard deviation, RSD)小于10%。结论 所建立的检测方法简便准确，可用于食品中新型非法添加物伐地那非杂质31的定性定量测定。 |
| 英文摘要: |
| Objective To establish a method for the determination of a new illegal additive in foods, vardenafil impurity 31 by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The UPLC-MS/MS was used to screen 92 kinds of substances of nafils illegally added in foods . The ultra performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS) was used to analyze the structure of the test sample. After the structure was inferred, the standard substance was purchased and verified. The target substance in the test sample was confirmed to be vardenafil impurity 31. The multiple reaction monitoring (MRM) method was established by UPLC-MS/MS, which was suitable for the qualitative and quantitative determination of vardenafil impurity 31 in foods. Results The limit of detection of vardenafil impurity 31 was 5 μg/kg, and the limit of quantitation was 10 μg/kg. The linear relationship was good in the linear range of 0.1-50.0 ng/mL, the correlation coefficient (r) was 0.9976, the average recovery rate was 85.33%-89.41%, and the relative standard deviation (RSD) was less than 10%. Conclusions The established method is simple and accurate, and can be used for the qualitative and quantitative determination of the new illegal additive vardenafil impurity 31 in foods. |
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