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目的:建立柱前衍生化RP-HPLC法测定夜宁颗粒中二苯乙烯苷含量的方法。方法:采用丹酰氯作为衍生化试剂,色谱柱为Wondasil-C8色谱柱(250 mm×4.6 mm,5μm),以(30 m M的乙酸铵用磷酸调节p H至3.5)-乙腈(78∶22)为流动相,柱温为30℃,流速为1.0 ml·min-1,荧光检测器检测(激发波长为370 nm,发射波长为560 nm),进样量为20μl。结果:制剂中其他成分无干扰,二苯乙烯苷在0.071~27.280 mg·ml-1范围内线性关系良好,r=0.999 9,平均回收率为99.04%,RSD为0.1%(n=9)。结论:所用方法简便快捷,灵敏度高,准确性好,可作为夜宁颗粒质量控制方法的依据。
OBJECTIVE: To establish a method for the determination of stilbene glycosides in YN granules by precolumn derivatization RP-HPLC. METHODS: Dansyl chloride was used as a derivatization reagent. The column was Wondasil-C8 (250 mm × 4.6 mm, 5 μm) with (30 μm M ammonium acetate adjusted to pH 3.5 with phosphoric acid) -acetonitrile (78:22 ) Was used as the mobile phase. The column temperature was 30 ℃, the flow rate was 1.0 ml · min-1, and the detection wavelength was 370 nm. The emission wavelength was 560 nm. The injection volume was 20 μl. Results: There was no interference in other components of the preparation. The calibration curve of stilbene glycoside was linear in the range of 0.071-27.280 mg · ml-1 with r = 0.999 9, the average recovery was 99.04% and the RSD was 0.1% (n = 9). Conclusion: The method used is simple, rapid, sensitive and accurate, which can be used as the basis for the quality control method of Ye-ning.