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目的:筛选巴豆油中佛波醇酯的水解工艺。方法:采用正交试验法,以水解时间、碱性甲醇用量、水解次数、温度为考察因素,佛波醇产率作为评价指标。采用Diamonsil C18分析柱(4.6 mm×250 mm,5μm),流动相乙腈-水(10∶90);检测波长234 nm;流速1 mL.min-1;柱温25℃;进样量20μL,测定佛波醇含量。结果:最佳水解时间10 h、碱性甲醇用量6倍量、水解次数1次及温度25℃。佛波醇在4.28～107 mg.L-1与峰面积间的线性关系良好,r=0.999 9,回收率为97.89%,RSD0.78%。结论:工艺稳定,结果准确,重复性好,可为佛波醇的进一步研究提供参考。
Objective: To screen the hydrolysis process of phorbol esters in croton oil. Methods: Using orthogonal test, the hydrolysis time, the amount of alkaline methanol, the number of hydrolysis, the temperature as the investigation factors, the phorbol yield as the evaluation index. Diamonsil C18 column (4.6 mm × 250 mm, 5 μm) was used. The mobile phase was acetonitrile-water (10:90). The detection wavelength was 234 nm. The flow rate was 1 mL.min-1. The column temperature was 25 ℃. Phorbol content. Results: The optimal hydrolysis time was 10 h, the amount of alkaline methanol was 6 times, the number of times of hydrolysis was 1 and the temperature was 25 ℃. The linear relationship of phorbol between 4.28 ~ 107 mg.L-1 and the peak area was good, r = 0.999 9, the recovery was 97.89% and the RSD was 0.78%. Conclusion: Stable process, accurate results and good repeatability can provide reference for the further study of phorbol.