强力枇杷露质量标准的提高和优化

Improvement and Optimization of Quality Standard for Qiangli Pipa Distillate Formula

目的:优化和提高强力枇杷露的质量标准。方法:删去原质量标准中的化学反应,应用TLC法对处方中的罂粟壳、枇杷叶和桔梗进行鉴别;用HPLC法测定来源于罂粟壳的吗啡和磷酸可待因的含量。吗啡含量测定色谱条件为:色谱柱:Inertsil ODS-3(250 mm×4.6 mm,5μm),流动相:乙腈-0.01 mol·L^(-1)庚烷磺酸钠溶液与0.02 mol·L^(-1)磷酸二氢钾溶液的等量混合液(用10%磷酸溶液调节p H至2.8)(13∶87),检测波长:220 nm,柱温:30℃,流速:1.0 ml·min^(-1);磷酸可待因含量测定色谱条件为:色谱柱:Inertsil ODS-3(250 mm×4.6 mm,5μm),流动相:乙腈-0.01 mol·L^(-1)庚烷磺酸钠溶液与0.02 mol·L^(-1)磷酸二氢钾溶液的等量混合液(用10%磷酸溶液调节p H至2.8)(15∶85),检测波长:220 nm,柱温:30℃,流速:1.0 ml·min^(-1)。结果:TLC法可用于鉴别罂粟壳、枇杷叶和桔梗;吗啡在3.14~62.80μg·ml^(-1)的浓度范围内线性关系良好(r=1.000 0),平均回收率96.69%(RSD=2.41%,n=9);磷酸可待因在3.52~87.94μg·ml^(-1)范围内线性关系良好(r=1.000 0),平均回收率为95.68%(RSD=2.64%,n=9)。结论:改进了强力枇杷露的质量标准,建立的方法操作简易、精密度和准确度都好、专属性也强。

Objective： To improve the quality standard for Qiangli Pipa distillate formula. Methods： The chemical reactions for identification in the old standard were deleted. TLC methods were established to identify Papaveris pericarpium,Eriobotryae folium and Platycodonis radix. The contents of morphine and codeine phosphate from Papaveris pericarpium were determined by HPLC. The chromatographic conditions for morphine content determination were as follows： an Inertsil ODS-3 chromatographic column（ 250 mm ×4. 6 mm,5 μ m） was used,the mobile phase was acetonitrile-the mixture of 0. 01 mol·L-1 sodium heptane sulfonate and 0. 02 mol·L-1 potassium dihydrogen phosphate with equal amount（ 10% phosphoric acid was used to adjust p H to 2. 8）（ 13 ∶87）,the detection wavelength was 220 nm,the column temperature was 30 ℃,and the flow rate was 1. 0 ml·min-1. The chromatographic conditions for codeine phosphate content determination were as follows ： an Inertsil ODS-3 chromatographic column（ 250 mm×4. 6 mm,5 μ m） was used,the mobile phase was acetonitrile-the mixture of 0. 01 mol · L-1 sodium heptane sulfonate and 0. 02 mol · L-1 s potassium dihydrogen phosphate with equal amount（ 10% phosphoric acid was used to adjust p H to 2. 8）（ 15 ∶85）,the detection wavelength was220 nm,the column temperature was 30 ℃,and the flow rate was 1. 0 ml· min-1. Results： TLC had obvious characteristics with clear and well-separated spots. Morphine showed a good linear relationship within the range of 3. 14-62. 8 μg·ml-1（ r=1. 000 0） with the average recovery of 96. 69%（ RSD = 2. 41%,n = 9）. Codeine phosphate showed a good linear relationship within the range of3. 52-87. 94 μg·ml-1（ r=1. 000 0） with the average recovery of 95. 68%（ RSD=2. 64%,n=9）. Conclusion： The quality standard for Qiangli Pipa distillate formula is improved. The methods are easy-operated and accurate with good specificity,which are suitable for the quality control of Qiangli Pipa distillate formula.