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目前山莨菪碱的质控方法有高氯醚滴定法和酸性染料比色法,二者在灵敏度和选择性方面都存在不足。采用HPLC,在色谱条件优化实验的基础上,以ZorbaxODS为固定相,流动相:甲醇-水-三乙胺(50:50:0.1,pH3.0),检测波长214nm,左旋咪唑为内标物。日内误差RSD=1.16%,日间误差RSD=1.44%。对山莨菪碱制剂进行的含量测定结果表明,该法具有操作简便、灵敏度高、分析速度快的优点,一次色谱分析过程6min即可完成。检测下限可达10ng,克服了以往文献中因流动相含乙醚、导致基线噪声过大,难于在近紫外区进行检测而损失了山莨菪碱响应灵敏度的缺陷。
At present, the methods for quality control of anisodamine include high-chloroether titration and acid dye colorimetry, both of which are insufficient in terms of sensitivity and selectivity. Using HPLC, on the basis of optimized chromatographic conditions, Zorbax ODS was used as the stationary phase, and the mobile phase was methanol-water-triethylamine (50:50:0.1, pH 3.0). The detection wavelength was 214 nm, and levamisole was used as the internal phase. Standard object. The intraday error RSD = 1.16%, and the daytime error RSD = 1.44%. The results of the determination of the anisodamine formulation showed that the method has the advantages of simple operation, high sensitivity, and high analysis speed. A chromatographic analysis process can be completed in 6 minutes. The detection limit can reach 10 ng, which overcomes the defect that the sensitivity of the anisodamine is lost because the mobile phase contains diethyl ether and the baseline noise is too large to detect in the near ultraviolet region.