论文部分内容阅读
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0.50~20μg/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0.2μg/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。
OBJECTIVE To establish a method for the determination of tert-butylhydroquinone (TBHQ) in fish oil soft capsule by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) The contents of 4 synthetic antioxidants including butylated hydroxytoluene (BHT), butyl hydroxyanisole (BHA) and propyl gallate (PG) were determined. Methods 152 batches of fish oil soft capsule were extracted with acetonitrile and vortex. UPLC was eluted with acetonitrile-water as mobile phase. The electrospray ionization (ESI-) and multi-reaction mass spectrometry Multiple reaction monitoring (MRM) was performed. Results PG, TBHQ, BHA and BHT had a good linearity (r> 0.997) in the concentration range of 0.50 ~ 20μg / mL. The recoveries were 88.8 at spiked levels of 3, 8, and 16 mg / kg % ~ 94.2%, RSD was 1.6% ~ 4.2% (n = 6), the detection limit was 0.2μg / kg. Conclusion The method has high sensitivity, good anti-interference and good accuracy. It can be applied to the detection of PG, TBHQ, BHA and BHT synthetic antioxidants in fish oil soft capsules.