高效液相色谱法检测食品中新型非法添加物双环己甲酰酚汀含量

Determination of the content of novel illegal additive dicyclohexylformylphentine in food by high performance liquid chromatography

中文关键词:  环己甲酰基取代酚汀  高效液相色谱  基质影响  违法添加

英文关键词:high performance liquid chromatography  dicyclohexylformylphentine  illegal addition

中文摘要:

      目的 建立高效液相色谱法检测食品中新型非法添加物双环己甲酰酚汀的方法。方法 采用乙腈作为提取溶剂, 提取液经色谱柱Waters Xbridge C18 (250 mm×4.6 mm, 5 μm)分离, 以乙腈+水为流动相进行等度洗脱, 外标法定量, 流速为1.0 mL/min, 检测波长为230 nm。结果 双环己甲酰酚汀在0.5~50.0 μg/mL质量浓度范围内的线性关系良好(r2 >0.9999), 检出限、定量限分别为1 mg/kg、5 mg/kg; 在梅子、固体饮料和压片糖果3种不同基质和1、2、10倍定量限的3个质控水平下的回收率在85.6%~99.2%, 相对标准偏差小于等于3.54%。将该方法用于评估某批次网抽阳性样品违法添加含量, 与超高效液相色谱-质谱法测定结果高度一致。结论 该方法简便、高效、准确, 适用于食品中违法添加双环己甲酰酚汀的快速检验。

英文摘要:

      Objective To establish a method for determination of the content of novel illegal additive dicyclohexylformylphentine in food by high performance liquid chromatography. Methods Acetonitrile was used as the extraction solvent, and the extraction solution was separated with a Waters Xbridge C18 (250 mm×4.6 mm, 5 μm) chromatographic column. Isocratic elution was carried out with acetonitrile+water as the mobile phase, and quantified by the external standard method. The flow rate was 1.0 mL/min and the detection wavelength was 230 nm. Results The dicyclohexylformylphentine had a good linear relationship within the mass concentration range of 0.5–50.0 μg/mL (r2>0.9999). The limit of detection and limit of quantitation were 1 mg/kg and 5 mg/kg, respectively. At 3 quality control levels of 1 times, 2 times and 10 times the limit of quantitation in 3 kinds of different matrices (plums, solid beverages and pressed candies), the recoveries ranged from 85.6% to 99.2%, with relative standard deviations less than or equal to 3.54%. This method was used to evaluate the illegal addition content of a batch of positive samples collected from online platforms, and the results were highly consistent with those determined by high performance liquid chromatography-mass spectrometry. Conclusion This method is simple, efficient and accurate, and is suitable for the rapid inspection of illegal additions of dicyclohexylformylphentine in food.