超高效液相色谱-串联质谱法测定鱼油软胶囊中的合成抗氧化剂

Determination of synthetic antioxidants in fish oil soft capsules 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  合成抗氧化剂  鱼油软胶囊

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  synthetic antioxidants  fish oil soft capsules

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)测定鱼油软胶囊中叔丁基对苯二酚(tert-butylhydroquinone, TBHQ)、2,6-二叔丁基-4-甲基苯酚(butylated hydroxytoluene, BHT)、丁羟基茴香醚(butyl hydroxyanisole, BHA)和没食子酸丙酯(propyl gallate, PG)4种合成抗氧化剂的含量。方法 采用乙腈为溶剂和涡旋方式对152批次鱼油软胶囊进行提取; UPLC以乙腈-水为流动相进行梯度洗脱, 质谱采用电喷雾离子源负离子模式(electrospray ionization, ESI-)及多反应监测模式(multiple reaction monitoring, MRM)进行测定。结果 PG、TBHQ、BHA和BHT在0.50~20 μg/mL浓度范围内具有良好的线性关系(r>0.997), 在2、8和16 mg/kg3个不同浓度加标水平下测得回收率为88.8%~94.2%, RSD为1.6%~4.2%(n=6), 检出限为0.2 μg/kg。结论 该方法灵敏度高、抗干扰性强且准确性好, 可适用于鱼油软胶囊中PG、TBHQ、BHA和BHT合成抗氧剂的检测。

英文摘要:

      Objective To establish a method for the determination of tert-butylhydroquinone (TBHQ), butylated hydroxytoluene (BHT), butyl hydroxyanisole (BHA) and propyl gallate (PG) in fish oil soft capsules by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Method Using acetonitrile as extraction solvent, 152 batches of fish oil soft capsules were handled with vortex mode. UPLC used acetonitrile and water as mobile phase for gradient elution, mass spectrometry used negative electrospray ionization mode (ESI-) and multiple reaction monitoring mode (MRM) for determination of PG, TBHQ, BHA and BHT. Results PG, TBHQ, BHA and BHT had good linear relationships in the range of 0.50~20 μg/mL with correlation coefficients more than 0.997. The recoveries spiked at 3 levels of 2, 8 and 16 mg/kg were 88.8%~94.2%, the relative standard deviations (RSD) were 1.6%~4.2% (n=6), and the limits of detection (LODs) were 0.2 μg/kg. Conclusions The method is sensitive, specific and accurate, which is suitable for the determination of synthetic antioxidants in fish oil soft capsules.