摘要
目的:建立柴胡药材活性成分含量的HPLC测定方法,考察钴60射线辐照前后活性成分含量的变化。方法:采用C_(18)色谱柱(4.6 mm×250 mm,5μm),流动相为0.1%磷酸水溶液-乙腈,梯度洗脱,流速1.0 m L·min^(-1),检测波长210 nm,柱温30℃。分别选择剂量为5、8、10 k Gy对柴胡药材进行辐照,比较辐照前后活性成分含量的变化,并进行成组t检验考察其显著情况。结果:柴胡皂苷a、c、d质量浓度分别在0.020~0.806、0.022~0.893及0.025~1.003 mg·m L^(-1)范围内有良好线性,平均加样回收率分别为99.4%、98.7%和99.8%;未经辐照的6批柴胡药材中柴胡皂苷a、c、d含量范围分别为3.023~3.245、1.034~1.341和5.023~5.298 mg·g^(-1);经10 k Gy辐照后,上述3个成分的含量范围分别为2.975~3.226、0.823~0.978和4.963~5.136 mg·g^(-1);经过5、8、10 k Gy辐照后,柴胡药材所含的成分柴胡皂苷a、c、d均有变化,经成组t-检验,在超过5 k Gy后,柴胡皂苷c辐照前后含量变化显著(P<0.01)。结论:所建立的柴胡活性成分测定方法可作为柴胡质控方法。在辐照剂量不超过5 k Gy时,各成分变化不显著,可为柴胡药材辐照灭菌手段提供参考。
Objective： To establish an HPLC method for determination of effective ingredients in Radix Bupleuri, and to investigate the effect of 60Co-γ ray irradiation on the effective components. Methods： The C18 column （ 4.6 mm × 250 mm, 5 μm ） was adopted and the mobile phase consisted of 0.1% acetic acid （ A ） and acetonitrile （ B ） with a gradient elution at the flow rate of 1.0 mL min-1, the wavelength of UV detection was 210 nm, and the column temperature was 30 ℃. Radix Bupleuri was irradiated at the dose of 5, 8 and 10 kGy. Then contents of the active ingredients before and after irradiation were compared by t-test. Results： The linear range of saikosaponin a, saikosaponin c and saikosaponin d were 0.020-0.806 mg mL-1, 0.022-0.893 mg mL-1 and 0.025-1.003 mg mL-1, respectively, and the average recoveries were 99.4%, 98.7% and 99.7%, respectively. The content ranges of saikosaponin a, saikosaponin c and saikosaponin d in 6 non-irradiated Radix Bupleuri were 3.023-3.245 mg g-l, 1.034-1.341 mg g-1 and 5.023-5.298 mg g-1, respectively; while the content ranges of those in the samples irradiated at 10 kGy were 2.975-3.226 mg g-l, 0.823-0.978 mg g-1 and 4.963-5.136 mg g-1, respectively. After irradiation at 5, 8 and 10 kGy, saikosaponin a, saikosaponin c and saikosaponin d in Radix Bupleuri changed. And significant difference was found between contents of saikosaponin c in samples irradiated at 5 kGy. Conclusion： The established method could be used in quality control of Radix Bupleuri. When the radiation was no more than 5 kGy, each active ingredient did not change significantly. The proposed method provided reference for sterilization of Radix Bupleuri.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2017年第6期1135-1141,共7页
Chinese Journal of Pharmaceutical Analysis
关键词
柴胡
钴60
柴胡皂苷
含量变化
辐照灭菌
保鲜技术
安全监测
高效液相色谱
Radix Bupleuri
60Co-γ ray
saikosaponin
content variation
radiant sterilization
keeping fresh
preservation technology
HPLC
