目的:检测醋酸奥曲肽注射剂中是否添加苯酚、苯甲醇、三氯叔丁醇、对羟基苯甲酸甲酯及对羟基苯甲酸丙酯5种抑菌剂。方法:采用C18(L)(4.6 mm×250 mm,5 μm)色谱柱,流动相A为水,流动相B为甲醇,梯度洗脱,流速为1.0 mL·min-1,柱温30℃,检测波长为220 nm及256 nm。结果:苯酚、苯甲醇、三氯叔丁醇、对羟基苯甲酸甲酯及对羟基苯甲酸丙酯各峰均分离良好;苯酚在1.29~258.60 μg·mL-1范围内线性关系良好(r=1.000),平均回收率为100.0%(n=9);苯甲醇在2.72~544.20 μg·mL-1范围内线性关系良好(r=0.9997),平均回收率为100.3%(n=9);三氯叔丁醇在9.95~1990.00 μg·mL-1范围内线性关系良好(r=1.000),平均回收率为100.9%(n=9);对羟基苯甲酸甲酯在0.27~53.80 μg·mL-1范围内线性关系良好(r=1.000),平均回收率为100.5%(n=9);对羟基苯甲酸丙酯在0.26~52.00 μg·mL-1范围内线性关系良好(r=1.000),平均回收率为99.4%(n=9);91批醋酸奥曲肽注射剂中均未检出5种抑菌剂。结论:该方法准确、灵敏、简便,可用于醋酸奥曲肽注射剂中苯酚、苯甲醇、三氯叔丁醇、对羟基苯甲酸甲酯及对羟基苯甲酸丙酯5种抑菌剂的检查。
Objective: To detect whether the octreotide acetate injection was added with the five antibacterial agents of phenol, benzyl alcohol, chlorobutanol, methyl p-hydroxybenzoate and propyl p-hydroxybenzoate. Methods: An Agela Venusuil ASB C18 (L) (4.6 mm×250 mm, 5 μm) column was adopted. The mobile phase A was water and the mobile phase B was methanol, the flow rate was 1.0 mL·min-1, the column temperature was 30℃, and the detection wavelength was 220 nm and 256 nm. Results: The five kinds of antibacterial agents were well separated. The linear range of phoenol was 1.29~258.60 μg·mL-1, and the average recovery was 100.0%(n=9). The linear range of benzyl alcohol was 2.72~544.20 μg·mL-1, and the average recovery was 100.3%(n=9). The linear range of chlorobutanol was 9.95~1990.00 μg·mL-1, and the average recovery was 100.9%(n=9). The linear range of methyl p-hydroxybenzoate was 0.27~53.80 μg·mL-1, and the average recovery was 100.5%(n=9). The linear range of propyl p-hydroxybenzoate was 0.26~52.00 μg·mL-1, and the average recovery was 99.4% (n=9). None of the five kinds of antibacterial agents were detected in the 91 batches of octreotide acetate injection. Conclusion: The method is accurate, sensitive and simple, and can be used for determination of phenol, benzyl alcohol, chlorobutanol, methyl p-hydroxybenzoate and propyl p-hydroxybenzoate in octreotide acetate injection.
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