HPLC测定口服液体制剂中防腐剂和甜味剂的含量

Content Determination of Preservatives and Sweeteners in Oral Liquid Preparations by HPLC

关键词:  口服液体制剂  防腐剂  甜味剂  高效液相色谱法  含量测定

Key words:  oral liquid preparation  preservatives  sweeteners  HPLC  content determination

摘要:

目的 建立快速定性定量检测口服液体制剂中违法添加防腐剂和甜味剂的高效液相色谱法。方法 ZORBAX SB-C₁₈色谱柱(4.6 mm×250 mm，5 μm)，流动相：甲醇-0.02 mol·L^-1乙酸铵溶液，梯度洗脱，流速：1.0 mL·min^-1，检测波长：240 nm，柱温：25 ℃。结果 安赛蜜、苯甲酸、山梨酸、糖精钠、脱氢乙酸、羟苯甲酯、羟苯乙酯、羟苯丙酯、羟苯丁酯在5~100 μg·mL^-1内线性关系良好(r>0.999)，检测限分别为0.02，0.04，0.01，0.10，0.06，0.01，0.01，0.01，0.01 μg·mL^-1，平均回收率在90.0%~110.0%内，精密度和重复性均<2.0%(n=6)。结论 该方法简单、可靠、准确，可用于口服液体制剂中防腐剂和甜味剂含量的测定。

Abstract:

OBJECTIVE To establish an HPLC method for determining the contents of preservatives and sweeteners in oral liquid preparations. METHODS The ZORBAX SB-C₁₈ chromatographic column(4.6 mm×250 mm, 5 μm) was adopted. The mobile phase was methanol-0.02 mol·L^-1 ammonium acetate solution with the gradient elution at the flow rate of 1.0 mL·min^-1. The detective wavelength was 240 nm, and the column temperature was 25 ℃. RESULTS Good resolution and linear correlation of acesulfame potassium, benzoic acid, sorbic acid, saccharin sodium, dehydroacetic, methylparaben, ethylparaben, propylparaben and butyl-p-hydroxybenzoate were found in the range of 5-100 μg·mL^-1(r>0.999). The detection limit of every components were 0.02, 0.04, 0.01, 0.10, 0.06, 0.01, 0.01, 0.01, 0.01 μg·mL^-1. The recovery range was 90.0%-110.0%. The instrument precision and repeatability were <2.0%(n=6). CONCLUTION This method is simple, reliable and accurate for determining the contents of preservatives and sweeteners in oral liquid preparation.