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目的:建立热感赛比斯坦颗粒定性定量方法。方法:采用薄层色谱法对热感赛比斯坦颗粒中罂粟壳、罂粟子、甘草、破布木果、蜀葵子、黄瓜子、榅桲子和巴旦仁进行定性鉴别;采用高效液相色谱法测定热感赛比斯坦颗粒中甘草苷、甘草酸铵和吗啡的含量。甘草苷和甘草酸铵含量测定色谱条件:采用Agilent TC C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈(A)-0.1%磷酸溶液(B)为流动相,梯度洗脱(0~10 min,19%A;10~15 min,19%A→25%A;15~30 min,25%A→38%A;30~42 min,38%A;42~50 min,38%A→19%A),流速1 m L·min-1,检测波长237 nm,柱温为30℃;吗啡含量测定色谱条件:采用Phenomenex Luna C8(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.5%醋酸铵水溶液(含三乙胺0.8%)(13∶87)为流动相,流速1.0 m L·min-1,检测波长286 nm,柱温30℃。结果:TLC斑点清晰,分离度好,阴性无干扰。甘草苷、甘草酸铵和吗啡质量浓度分别在3.68~73.64、18.62~260.68和5.33~85.28μg·m L-1范围内,与峰面积线性关系良好,r分别为0.999 8、0.999 9和0.999 8);平均回收率(n=6)分别为102.9%、102.2%和99.71%,RSD分别为0.98%、1.4%和1.7%。结论:所建方法可用于热感赛比斯坦颗粒的质量控制。
Objective: To establish a qualitative and quantitative method for heat-sensitive cystamine particles. Methods: The contents of poppy, poppy, licorice, ragweed, holly berberis, cucumber, razor clam, and barren kernel in the heat-sensitive cystatin granules were qualitatively identified by TLC. Method to determine the content of liquiritigenin glycyrrhizinate, glycyrrhizinate and morphine in the heat-sensitive cystatin granules. Determination of Liquiritin and Ammonium Glycyrrhizinate Chromatographic conditions: The mobile phase was eluted with acetonitrile (A) -0.1% phosphoric acid (B) with gradient elution on a Agilent TC C18 (250 mm × 4.6 mm, 5 μm) 10 min, 19% A; 10-15 min, 19% A → 25% A; 15-30 min, 25% A → 38% A; 30-42 min, 38% A; → 19% A) at a flow rate of 1 m L · min-1 at a detection wavelength of 237 nm with a column temperature of 30 ° C .; determination of morphine content chromatographic conditions: a Phenomenex Luna C8 (250 mm × 4.6 mm, 5 μm) Aqueous 0.5% ammonium acetate solution (containing triethylamine 0.8%) (13:87) was used as the mobile phase at a flow rate of 1.0 mL · min-1. The detection wavelength was 286 nm and the column temperature was 30 ℃. Results: TLC spots clear, good resolution, negative non-interference. The concentrations of glycyrrhizin, ammonium glycyrrhizinate and morphine were in the range of 3.68-73.64, 18.62-260.68 and 5.33-85.28μg · m L-1, respectively, with a good linear relationship with the peak area, with r values of 0.999 8, 0.999 9 and 0.999 8 ). The average recoveries (n = 6) were 102.9%, 102.2% and 99.71%, respectively, with RSDs of 0.98%, 1.4% and 1.7%, respectively. Conclusion: The proposed method can be used for the quality control of heat-sensitive cystamine particles.