HPLC内标法测定蜂蜜中抗生素的研究

Study on Antibiotics in Honey by HPLC Internal Standard Method

建立了蜂蜜中检测三种抗生素（土霉素、四环素、甲硝唑）的内标定量方法,考察了样品萃取液中三氟乙酸-甲醇、磷酸二氢钠-甲醇、草酸-甲醇、盐酸-甲醇、甲醇等五种溶液对提取率的影响,结果表明盐酸-甲醇溶液对三种抗生素的提取率最高.流动相由甲醇和0.002 mol·L-1草酸组成,梯度洗脱,流速为0.8 mL·min-1.该方法在10～200 μg·g-1内线性关系良好,加标回收率为82.4％～93.7％,该方法可用于蜂蜜中三种抗生素的微量检测,该方法用于20种市售蜂蜜的检测,其中85％呈阳性.

HPLC internal standard method was established to determine three kinds of antibiotic in honey. The effect of extracting solution on recovery rate was investigated between methanol solution with triflurine formic acid, sodium dihydrogen phosphate, oxalic acid, hydrochloric acid respectively, which displayed that extracting solution from methanol and hydrochloric acid present the highest recovery rate. Mobile phase consisted of methanol and 0.002 mol.L1 oxalic acid, the flow rate of gradient elution was 0.8 mL.min-1 .This method with the good linearity between 10-200 μg.g-1 and the lower limits of quantification can be used for the analysis of three kinds of antibiotics in acne products. 20 kinds of acne products was analyzed in this way, and the antibiotics of 85 % product present positive.