超高效液相色谱-串联质谱法测定火锅底料中63种工业染料和5种生物碱类药物残留

Determination of 63 kinds of industrial dyes and 5 kinds of alkaloids drug residues in hot pot by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  火锅底料  工业染料  生物碱  

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  hot pot  industrial dyes  alkaloids

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)检测火锅底料中63种工业染料和5种生物碱类药物残留的方法。方法 样品经80%乙腈提取, 玻璃纤维滤纸除脂肪和蛋白质, 采用Phenomenex Kinetex F5色谱柱(2.1 mm×100 mm, 2.6 μm)分离, 以乙腈和5 mmmol/L甲酸铵水溶液作为流动相进行梯度洗脱, 采用电喷雾离子源, 正/负离子多反应监测。结果 68种化合物在一定质量浓度范围内线性关系良好, 相关系数(r2)≥0.99590; 检出限为1.0~5.0 μg/kg, 定量限为2.0~10.0 μg/kg, 回收率范围为72.4%~109.2%, 相对标准偏差为1.2%~9.2% (n=6)。结论 本研究简单高效, 适用于火锅底料中63种工业染料和5种生物碱类药物的测定, 该方法显著提升了检测效率和结果准确性, 为食品安全监管提供了有力的技术支撑。

英文摘要:

      Objective To establish a method for determination of 63 kinds of industrial dyes and 5 kinds of alkaloids drug residues in hot pot by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was extracted with 80% acetonitrile, and the fat and proteins were removed using glass fiber filter paper, and separated with Phenomenex Kinetex F5 column (2.1 mm×100 mm, 2.6 μm). A gradient elution was performed using acetonitrile and 5 mmol/L ammonium formate in water as the mobile phase. Data were acquired in multiple reaction monitoring mode using electrospray ionization in dual polarity (positive/negative ion mode). Results The study confirmed that good linearity (r2>0.99590) was observed within a certain mass concentration range. The limits of detection were 1.0–5.0 μg/kg, and the limits of quantitation were 2.0–10.0 μg/kg. Recovery rates were 72.4%–109.2% with relative standard deviations of 1.2%–9.2% (n=6). Conclusion This study developes a simple and efficient method for the simultaneous determination of 63 kinds of industrial dyes and 5 kinds of alkaloid drugs in hot pot seasonings. The proposed approach significantly improves detection efficiency and result accuracy, providing robust technical support for food safety regulation.