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目的:建立UPLC法同时测定钩藤提取物中钩藤碱、异钩藤碱、去氢钩藤碱、异去氢钩藤碱的含量。方法:采用BEH C18色谱柱(100 mm×2.1 mm,1.7μm);以5 mmol/L醋酸铵缓冲液(0.01%氨水调p H=9)(A)-甲醇(B)-乙腈(C)三元体系为流动相进行梯度洗脱;流速:0.44 m L/min;柱温:30℃;检测波长:245 nm。结果:钩藤碱、异钩藤碱、去氢钩藤碱、异去氢钩藤碱的质量浓度在2.97~296.67μg/m L、1.31~450.00μg/m L、1.58~433.33μg/m L、1.28~438.33μg/m L的范围内线性关系良好,r为0.9993~0.9995;各成分平均加样回收率在97.34%~101.85%,RSD≤2.65%。钩藤提取物中钩藤碱、异钩藤碱、去氢钩藤碱、异去氢钩藤碱的含量分别为23.48、6.19、6.73、9.22μg/g。结论:该方法准确可靠,便于操作,可用于同时测定钩藤提取物中4种生物碱的含量。
OBJECTIVE: To establish a simultaneous UPLC method for the determination of rhynchophylline, isoniagluran, rhynchophylline and isorhamnetin in Uncaria rhynchophylla. METHODS: The samples were separated on a BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with 5 mmol / L ammonium acetate buffer (0.01% ammonia water and p H = 9) The ternary system was used as the mobile phase for gradient elution; the flow rate was 0.44 m L / min; the column temperature was 30 ℃; the detection wavelength was 245 nm. Results: The concentrations of rhynchophylline, isoniagluran, rhynchophylline and isorhamine were 2.97 ~ 296.67μg / m L, 1.31 ~ 450.00μg / m L, 1.58 ~ 433.33μg / m L , 1.28 ~ 438.33μg / m L within a good linear relationship, r was 0.9993 ~ 0.9995; average recovery of each component was 97.34% ~ 101.85%, RSD ≤ 2.65%. The contents of rhynchophylline, isorhamnetine, rhynchophylline and isorhamnetin in Uncaria macrophylla extract were 23.48, 6.19, 6.73 and 9.22μg / g, respectively. Conclusion: The method is accurate and reliable, easy to operate, and can be used for simultaneous determination of four alkaloids in Uncaria ramosissima extract.