高效液相色谱法测定芝麻油中的叔丁基羟基茴香醚、2,6-二叔丁基对甲酚、特丁基对苯二酚

Determination of tert-butyl hydroxyanisole, 2, 6-di-tert-butyl paracresol and tert-butyl hydroquinone in sesame oil by high performance liquid chromatography

建立高效液相色谱法测定芝麻油中叔丁基羟基茴香醚(BHA)、2,6-二叔丁基对甲酚(BHT)、特丁基对苯二酚(TBHQ)的含量。用25mL甲醇分5次涡旋超声提取芝麻油中的BHA,BHT,TBHQ,以La ChromC18(250mm×4.6mm,5μm)为色谱柱,以甲醇-0.5%甲酸水溶液为流动相进行梯度洗脱,流量为1.0mL/min,进样体积为5μL,柱温为35℃,检测波长为280nm。BHA,BHT,TBHQ的质量浓度在20~300mg/L范围内与其色谱峰面积呈良好的线性关系,相关系数大于0.999,方法检出限为0.5~1.0mg/kg。样品加标回收率为95.1%~99.8%,测定结果的相对标准偏差为2.1%~4.7%(n=6)。该方法操作简单,试剂用量少,准确度高,精密度好,适用于芝麻油中BHA,BHT,TBHQ含量的日常检测。

The HPLC method was established for the determination of tert-butyl hydroxyanisole(BHA),2,6-ditert- butyl paracresol(BHT) and tert-butyl hydroquinone(TBHQ) in sesame oil.BHA,BHT and TBHQ in sesame oil were extracted by 25 mL methanol with 5-time vortex ultrasound.The La Chrom C18 column (250 mm×4.6 mm,5 μm) was used as chromatographic column,and the gradient elution with methanol-0.5% formic acid aqueous solution as tmobile phase.The flow rate was 1.0 mL/min,the injection volume was 5 μL,the column temperature was 35℃,and the detection wavelength was 280 nm.The mass concentration of BHA,BHT and TBHQ had good linear relationship with the chromatographic peak area in the range of 20-300 mg/L.The correlation coefficients were greater than 0.999,the detection limits were 0.5-1.0 mg/kg.The recoveries were 95.1%-99.8%,and the relative standard deviations of the determination results were 2.1%-4.7%(n=6).The method is simple in operation,with less reagent,high accuracy and good precision.It is suitable for routine determination of BHA,BHT and TBHQ in sesame oil.