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目的:对颠茄口服溶液原质量标准中的鉴别和含量测定方法进行改进。方法:制备HPLC特征图谱来鉴别颠茄口服溶液;用HPLC双波长法同时测定颠茄口服溶液中东莨菪内酯和硫酸天仙子胺的含量。指纹图谱采用Waters Sun Fire C_(18)(250mm×4.6 mm,5μm)色谱柱,流动相为甲醇和0.05%磷酸溶液梯度洗脱,流速为1.0 ml·min~(-1),检测波长344 nm,柱温30℃;东莨菪内酯和硫酸天仙子胺的含量测定采用相同的C_(18)色谱柱,流动相为10 mmol·L~(-1)庚烷磺酸钠溶液(用冰醋酸调pH至3.3)-无水乙醇-乙腈(68.75∶6.25∶25),流速为1.0 ml·min~(-1),检测波长为344 nm和210 nm,柱温30℃。结果:颠茄口服溶液的特征图谱和颠茄酊原料的特征图谱一致,各特征峰和参照峰(东莨菪内酯峰)的保留时间及相对峰面积符合中国药典要求。在含量测定条件下,东莨菪内酯和硫酸天仙子胺与相邻的杂质峰完全分离,两者的浓度分别在5.168~103.360μg·ml~(-1)(r=1.000 0)和50.560~758.400μg·ml~(-1)(r=0.999 9)范围内线性关系良好;平均回收率分别为101.79%(RSD=1.05%,n=6)、100.92%(RSD=0.97%,n=6)。结论:改进后的质量控制方法,鉴别试验专属性强,含量测定选择两个指标性成分,更能全面控制颠茄口服溶液的质量,测定方法操作简便,准确,可为其质量控制提供可靠的方法。
OBJECTIVE: To improve the method of identification and content determination of the original quality standard of belladonna oral solution. METHODS: The HPLC profile was used to identify the belladonna oral solution. The content of scopoletin and cefazolin sulfate in the belladonna oral solution was simultaneously determined by HPLC dual wavelength method. The fingerprint was eluted with a gradient of methanol and 0.05% phosphoric acid using a Waters Sun Fire C 18 (250 mm × 4.6 mm, 5 μm) column with a flow rate of 1.0 ml · min -1 and a detection wavelength of 344 nm The column temperature was 30 ℃. The content of scopoletin and cefazolin sulfate was determined by the same C 18 column with a mobile phase of 10 mmol·L -1 sodium heptanesulfonate (using glacial acetic acid The pH was adjusted to 3.3) - ethanol - acetonitrile (68.75:6.25:25) at a flow rate of 1.0 ml · min -1. The detection wavelength was set at 344 nm and 210 nm with a column temperature of 30 ℃. Results: The characteristic map of belladonna oral solution was consistent with the characteristic map of belladonna tincture raw material. The retention time and relative peak area of each characteristic peak and reference peak (scopoletin peak) conformed to the requirement of Chinese Pharmacopoeia. Scopolactone and cefotaxime sulfate were completely separated from the adjacent impurity peaks under the conditions of content determination. The concentrations of scopolactone and sulfanilic acid were completely separated from each other at 5.168 ~ 103.360μg · ml -1 (r = 1.000 0) and 50.560 ~ The average recoveries were 101.79% (RSD = 1.05%, n = 6), 100.92% (RSD = 0.97%, n = 6) in the range of 758.400μg · ml -1 (r = 0.999 9) ). CONCLUSION: The improved quality control method, the high specificity of the identification test and the selection of the two index components make it possible to control the quality of the oral solution of belladonna. The method is simple, accurate and reliable, and can provide reliable quality control method.