用RP-HPLC法测定心肌保护液中盐酸普鲁卡因及其降解产物对氨基苯甲酸的含量

Determination of contents of procaine hydrochloride and its degradation product p-amino benzoic acid in myocardial preservation solution by RP-HPLC method

目的:建立RP-HPLC法测定心肌保护液中盐酸普鲁卡因及其降解产物对氨基苯甲酸含量。方法:采用Hyper-silC18柱(200mm×4.6mm,5μm),流动相为乙腈-0.05mol/L磷酸二氢钾溶液(内含0.005mol/L庚烷磺酸钠,用磷酸调pH至3.0)15:85,以氢溴酸加兰他敏为内标,检测波长283nm,流速0.8mL/min。结果:心肌保护液中盐酸普鲁卡因在0.25～32μg/mL内呈良好线性关系(r=0.9999),降解产物对氨基苯甲酸在0.025～3.2μg/mL内呈良好线性关系(r=0.9999)。盐酸普鲁卡因3.20、3.84、4.80μg/mL的回收率分别为(101.5±0.70)%、(101.3±0.49)%和(104.0±0.69)%。对氨基苯甲酸0.16、0.20、0.24μg/mL的回收率分别为(103.6±1.76)%、(102.2±1.70)%和(100.9±1.11)%(n=3)。结论:本方法可用于心肌保护液中盐酸普鲁卡因和降解产物对氨基苯甲酸的含量测定。

Objective：To establish a RP HPLC method for determining the contents of procaine hydrochloride and its degradation product p-amino benzoic acid in myocardial preservation solution. Methods： Procaine hydrochloride, p-amino benzoicacid and the internal standard galantamine hydrobromide were separated on a Hypersil C18 column（200 min×4.6 mm, 5μm）.The mobile phase was acetonitrile-0.05 mol/L potassium dihydrogen phosphate （including 0. 005 mol/L sodium heptane sulfon ic acid,adjusted to pH 3.0 with phosphoric acid） 15 ： 85. The detection wavelength was 283 nm. The flow rate was 0.8 mL/min. Results：Procaine hydrochloride presented a good linear relationship in the range of 0.25-32 μg/mL（r： 0. 999 9） ;p-amino benzoic acid also had a good linearity in the range of 0. 025-3.2 p.g/mL（r=0. 999 9）. The recovery rates of procaine hydrochloride at the concentrations of 3.20,3.84 and 4.80 /lg/mL were （101.5±0.70）%,（101.3±0.49）% and （104.0±0.69）%（n=3）, respectively. The recovery rates of p-amino benzoic acid at concentrations of 0.16,0.20 and 0.24 μg/mL were （103.6±-4- 1.76）%, （ 102.2 ± 1.70） % and （ 100.9 ± 1. 11 ） % （ n = 3 ）, respectively. Conclusion ： The method is suitable for quantitative de- termination of contents of procaine hydroehloride and its degradation product p-amino benzoic acid in myocardial preservation solution.