气相色谱-串联质谱法检测肉类中16种氟代液晶化合物含量

Determination of the content of 16 kinds of fluorinated liquid-crystal compounds in meats by gas chromatography-tandem mass spectrometry

中文关键词:  同位素内标  气相色谱-串联质谱法  氟代液晶化合物  肉类

英文关键词:isotope labeling  gas chromatography-tandem mass spectrometry  fluorinated liquid-crystal compounds  meat

中文摘要:

      目的 建立气相色谱-串联质谱法测定肉类(猪肉、牛肉、羊肉和鸡肉)中16种氟代液晶化合物含量的方法。方法 样品经正己烷/二氯甲烷(1:1, V:V)超声提取后, 经弗罗里硅土固相萃取柱净化, 再经DB-5MS气相色谱柱分离, 采用大气压化学电离源正离子模式, 以气相色谱-串联质谱法进行多反应监测, 内标法定量。结果 16种氟代液晶化合物在0.1~50.0 μg/L范围内线性关系良好, 相关系数大于0.995, 检出限为0.02~0.18 μg/kg, 定量限为0.07~0.59 μg/kg。3个加标水平(1.0、10.0、50.0 μg/kg)的回收率为86.3%~113.7%, 相对标准偏差为1.4%~11.2%。结论 该方法前处理简单、快速、准确、灵敏, 适用于肉类食品中氟代液晶化合物的定性和定量检测, 可以为肉类食品的质量安全筛查提供方法参考与技术支撑。

英文摘要:

      Objective To establish a method for the determination of 16 kinds of fluorinated liquid-crystal compounds in meats including pork, beef, lamb and chicken by gas chromatography-tandem mass spectrometry. Methods After ultrasonic extraction with N-hexane/dichloromethane (1:1, V:V), the samples were purified via Florisil solid-phase extraction column, and then separated by DB-5MS gas chromatographic column. Atmospheric pressure chemical ionization source in positive ion mode was adopted, and multiple reaction monitoring was performed by gas chromatography-tandem mass spectrometry with internal standard method for quantitative analysis. Results The linear relationship of the 16 kinds of fluorinated liquid-crystal compounds was good within the range of 0.1–50.0 μg/L, and the correlation coefficient was greater than 0.995. The limits of detection were 0.02–0.18 μg/kg, and the limits of quantitation were 0.07–0.59 μg/kg. At the spiked levels of 1.0, 10.0 and 50.0 g/kg, the recoveries ranged from 86.3% to 113.7%, the relative standard deviations were 1.4%–11.2%. Conclusion The method is simple, quick, accurate and sensitive. It is suitable for the confirmation and quantification of fluorinated liquid-crystal compounds in meat samples. This method can provide a reference and technical support for the quality and safety screening of meat samples.