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目的:建立炒芥子配方颗粒的质量标准。方法:采用TLC法对芥子进行定性鉴别;采用HPLC法,对方中芥子碱硫氰酸盐进行含量测定,色谱柱为Hibar Purospher STAR C_(18)(250 mm×4.6 mm,5μm),流动相:以乙腈-0.08 mol·L~(-1)磷酸二氢钾(10∶90),流速:1 ml·min~(-1),柱温:35℃,检测波长:326 nm。结果:TLC法中炒芥子配方颗粒在与芥子碱硫氰酸盐对照品相应位置上,显相同颜色的斑点且斑点清晰;芥子碱硫氰酸盐线性范围为0.012 2~3.912 3μg,r=0.999 9;平均回收率为100.4%,RSD=0.6%(n=6);炒芥子配方颗粒水分、溶化性、粒度均符合要求。结论:本研究建立的定性及定量方法简单可行,重复性好,可用于炒芥子配方颗粒的质量控制。
Objective: To establish the quality standard of fried mustard seed. Methods: The mustard was identified qualitatively by TLC method. The content of the sinapine thiocyanate was determined by HPLC. The column was Hibar Purospher STAR C 18 (250 mm × 4.6 mm, 5 μm) With acetonitrile-0.08 mol·L -1 potassium dihydrogen phosphate (10:90), the flow rate was 1 ml · min -1, the column temperature was 35 ℃ and the detection wavelength was 326 nm. Results: In the TLC method, the particles of the fried mustard seeds showed the same color spots and clear spots at the corresponding positions of the control sample of sinapine thiocyanate. The linear range of the sinapine thiocyanate was 0.012 2 ~ 3.912 3 μg, r = 0.999 9; the average recovery was 100.4% and the RSD was 0.6% (n = 6). The water content, solubility and particle size of the fried mustard seed were both satisfactory. Conclusion: The qualitative and quantitative methods established in this study are simple and feasible with good repeatability and can be used for the quality control of fried mustard seed.