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目的:建立高效液相色谱法同时测定药用丁基胶塞中的抗氧剂264、抗氧剂1010和抗氧剂5057。方法:采用HPLC法对抗氧剂264(2,6-二叔丁基-4-甲基苯酚)、抗氧剂1010{四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯}和抗氧剂5057(丁基或辛基取代的二苯胺)的迁移量进行研究;使用Inertsil ODS C_(18)色谱柱(4.6 mm×150 mm,5μm),以甲醇为流动相A,10 mmol·L~(-1)乙酸铵溶液为流动相B,梯度洗脱,流速1.0 m L·min~(-1),检测波长220 nm(检测抗氧剂264和抗氧剂1010)、280 nm(检测抗氧剂5057);利用LC-MS/MS方法进行鉴别,采用三重四极杆质谱检测器、电喷雾离子源ESI,以正负离子模式扫描,质量数扫描范围m/z 50~1 500。结果:浸提试验确证了胶塞中含有的抗氧剂。几种抗氧剂的分离度良好,抗氧剂5057无明显降解产物,抗氧剂264与抗氧剂1010的降解产物均能与各自主峰分开,抗氧剂264、1010、5057的检出限分别为0.081、0.061、0.062μg·m L~(-1),且在各自的线性范围内线性关系良好(r=0.999 6~0.999 9,n=5),平均回收率均在98%~102%。5个企业的20批样品中均未检出抗氧剂。结论:建立的方法可用于对胶塞中抗氧剂264、1010、5057进行迁移研究。
Objective: To establish a HPLC method for the simultaneous determination of antioxidant 264, antioxidant 1010 and antioxidant 5057 in butyl butyl rubber stopper. Methods: Antioxidant 264 (2,6-di-tert-butyl-4-methylphenol) and antioxidant 1010 {tetrakis [β- ) Propionate] and anti-oxidant 5057 (butyl or octyl substituted diphenylamine) were investigated by using the mobile phase of Inertsil ODS C 18 column (4.6 mm × 150 mm, 5 μm) As mobile phase A, 10 mmol·L -1 ammonium acetate solution was used as mobile phase B, gradient elution was performed at a flow rate of 1.0 mL · min -1 and the detection wavelength was set at 220 nm (anti-oxidant 264 and anti- Oxygen reagent 1010), 280 nm (detection of antioxidant 5057); using LC-MS / MS method to identify the use of triple quadrupole mass spectrometer detector ESI electrospray ionization mode to scan the mass scan range m / z 50 ~ 1 500. Results: Leaching tests confirmed the antioxidant contained in the stopper. The separation of several antioxidants is good, antioxidant 5057 no obvious degradation products, antioxidants 264 and antioxidant 1010 degradation products can be separated from the main peak, the detection limit of antioxidant 264,1010,5057 (R = 0.999 6 ~ 0.999 9, n = 5), and the average recoveries were in the range of 98% ~ 102 %. Antioxidants were not detected in 20 batches of samples from 5 companies. Conclusion: The established method can be used to study the migration of antioxidant 264,1010,5057 in rubber stopper.