60Co-γ射线辐照灭菌对香砂枳术丸中5种有效成分的影响

Effect of 60Co-γ Ray Irradiation on Five Active Ingredients in Xiangshazhizhu Pills

关键词:  香砂枳术丸  ⁶⁰Co-γ射线  木香烃内酯  去氢木香烃内酯  柚皮苷  橙皮苷  新橙皮苷

Key words:  Xiangshazhizhu pills  ⁶⁰Co-γ ray  costunolide  dehydrocostuslactone  naringin  hesperidin  neohesperidin

摘要:

目的 建立同时测定香砂枳术丸中木香烃内酯、去氢木香烃内酯、柚皮苷、橙皮苷及新橙皮苷5种活性成分含量的测定方法，考察⁶⁰Co-γ射线辐照前后有效成分含量的变化。方法 采用Agilent-C₁₈色谱柱（4.6 mm×250 mm，5 μm），流动相为乙腈-0.5%磷酸溶液，梯度洗脱，检测波长为225 nm，流速为1.0 mL·min^-1，柱温为35℃。分别选择辐照剂量2，5，8 kGy对香砂枳术丸进行辐照，测定辐照前后香砂枳术丸中5种有效成分的含量，并进行成组t-检验考察其显著情况。结果 木香烃内酯、去氢木香烃内酯、柚皮苷、橙皮苷及新橙皮苷分别在0.060 6~3.032 5，0.025 8~1.290 0，0.037 3~1.865 0，0.044 2~2.210 0及0.033 6~1.680 0 μg内有良好线性，平均加样回收率分别为100.6%，101.0%，99.7%，100.2%和99.5%，RSD分别为0.5%，1.3%，0.8%，1.0%和0.7%。经过2，5，8 kGy辐照后，香砂枳术丸所含的有效成分木香烃内酯、去氢木香烃内酯、柚皮苷、橙皮苷及新橙皮苷均有变化，经成组t-检验，在>5 kGy后，木香烃内酯及去氢木香烃内酯辐照前后含量有统计学意义（P<0.05）。结论 所建立的香砂枳术丸活性成分测定方法回收率高、重复性好、简单实用，可作为香砂枳术丸质控方法。在辐照剂量≤ 5 kGy时，各成分变化不显著，为香砂枳术丸辐照灭菌手段提供了参考。

Abstract:

OBJECTIVE To establish a method to determine the content of 5 active ingredinents of costunolide, dehydrocostuslactone, naringin, neohesperidin and hesperidin in Xiangshazhizhu pills, and investigate the changes of the content of effective ingredinents before and after ⁶⁰Co-γ ray irradiation. METHODS The Agilent-C₁₈ column(4.6 mm×250 mm, 5 μm) was adopted and the detection wavelength was 225 nm with the flow rate of 1.0 mL·min^-1. The mobile phase was consisted of acetonitrile-0.5% phosphoric acid with a gradient elution, and column temperature was 35℃. The irradiation dose of 2, 5 and 8 kGy were selected to irradiate Xiangshazhizhu pills, and the content of 5 active ingredinents in Xiangshazhizhu pills before and after irradiation was compared, and the significant situation was observed by group t-test. RESULTS The linear range of costunolide, dehydrocostuslactone, naringin, hesperidin and neohesperidin were 0.060 6-3.032 5, 0.025 8-1.290 0, 0.037 3-1.865 0, 0.044 2-2.210 0 and 0.033 6-1.680 0 μg, and the average recovery were 100.6%, 101.0%, 99.7%, 100.2% and 99.5%, RSD were 0.5%, 1.3%, 0.8%, 1.0% and 0.7%. After irradiation of 2, 5 and 8 kGy, the effective ingredinents of costunolide, dehydrocostuslactone, naringin, hesperidin and neohesperidin were changed. Over 5 kGy, costunolide and dehydrocostuslactone according to change of content before and after irradiation was statistically significant(P<0.05) by group t-test. CONCLUSION The established method has a high recovery rate, good repeatability, is simple and practical and can be used for quality control for Xiangshazhizhu pills. When the radiation dose is ≤ 5 kGy, the changes of each component are not significant, which can provide a reference for the sterilization of Xiangshazhizhu pills.