不同剂量⁶⁰Co-γ射线辐照对二妙丸中6个有效成分影响的研究

目的：建立同时测定二妙丸中苍术素、苍术素醇、盐酸小檗碱、盐酸药根碱、盐酸黄柏碱和盐酸巴马汀6个有效成分含量的测定方法，考察不同剂量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&#215;250 mm，5 μm），以乙腈（A）-0.5%磷酸水溶液（B）（每100 mL加十二烷基硫酸钠0.2 g）为流动相进行梯度洗脱，检测波长分别为280 nm和340 nm，流速1.0 mL&#183;min^-1，柱温28℃。分别选择辐照剂量为2、5、8 kGy对二妙丸进行辐照，比较辐照前后二妙丸中6个有效成分含量的变化，并进行成组t检验考察其显著情况。结果：苍术素、苍术素醇、盐酸小檗碱、盐酸药根碱、盐酸黄柏碱和盐酸巴马汀分别在0.090 1~2.252 5、0.128 9~3.222 5、0.246 5~6.162 5、0.076 8~1.920 0、0.120 3~3.007 5及0.051 2~1.280 0范围内有良好线性，平均加样回收率分别为99.6%、99.7%、100.5%、98.8%、101.4%及99.1%，RSD分别为1.2%、0.60%、0.50%、0.90%、1.0%和0.80%。经过2、5、8 kGy辐照后，二妙丸所含的有效成分苍术素、苍术素醇、盐酸小檗碱、盐酸药根碱、盐酸黄柏碱和盐酸巴马汀均有变化，经成组t-检验，在超过5 kGy后，苍术素及苍术素醇辐照前后含量变化显著（P<0.05）。结论：所建立的二妙丸活性成分测定方法准确，重复性好，简单实用，可作为二妙丸质控方法。在辐照剂量不超过5 kGy时，各成分变化不显著，为二妙丸辐照灭菌提供了参考。

Objective:To establish an HPLC method for simultaneous determination of 6 active ingredients (atractylodin,atractyoldinol,berberine hydrochloride,jatrorrhizine hydrochloride,phellodendrine hydrochloride and palmatine hydrochloride) in Ermiao pills,and to investigate the effect of ⁶⁰Co-γ ray irradiation on the effective components. Methods:The Agilent-C₁₈ column(4.6 mm&#215;250 mm,5 μm) was adopted and the wavelength of UV detection was 280 nm and 340 nm with the flow rate of 1.0 mL&#183;min^-1. The mobile phase consisted of acetonitrile (A)-0.5% phosphoric acid (B) (containing 0.2 g of sodium dodecyl sulfate per 100 mL) with a gradient elution. The column temperature was 28℃. Doses for irradiation on Ermiao pills were 2 kGy,5 kGy and 8 kGy. The contents of 6 active ingredients before and after irradiation were compared,and a t-test study was used to examine the significance. Results:The linear ranges of atractylodin,atractyoldinol,berberine hydrochloride,jatrorrhizine hydrochloride,phellodendrine hydrochloride and palmatine hydrochloride were 0.090 1-2.252 5 μg,0.128 9- 3.222 5 μg,0.246 5-6.162 5 μg,0.076 8-1.920 0 μg,0.120 3-3.007 5μg and 0.051 2-1.280 0 μg,and the average recovery were 99.6%,99.7%,100.5%,98.8%,101.4% and 99.1% with RSDs of 1.2%,0.60%,0.50%,0.90%,1.0% and 0.80%.After irradiation at doses of 2 kGy,5 kGy and 8 kGy,the contents of atractylodin,atractyoldinol,berberine hydrochloride,jatrorrhizine hydrochloride,phellodendrine hydrochloride and palmatine hydrochloride all changed. Results of group t-test indicated significant change (P<0.05) of contents of atractylodin and atractyoldinol after irradiation at doses above 5 kGy. Conclusion:The established method is accurate,repeatable,simple and practical,and can be used for quality control of Ermiao pills. When the radiation dose is below 5 kGy,the changes of each component are not significant,which provides a reference for the sterilization of Ermiao pills.

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