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作 者:张梦晨 谢辉[1] 何畅 毛春芹[1] 张奕雯 邹梦恬 Zhang Mengchen;Xie Hui;He Chang;Mao Chunqin;Zhang Yiwen;Zou Mengtian(College of Pharmacy,Nanjing University of Chinese Medicine,Nanjing 210023,China)
出 处:《中国药师》2020年第9期1696-1699,1780,共5页China Pharmacist
基 金:国家重点研发计划项目(编号:2018YFC1707000);江苏高校品牌专业建设工程项目(编号:PPZY2015A070)。
摘 要:目的:建立山药饮片HPLC指纹图谱,通过研究不同剂量60Co-γ射线辐照前后HPLC指纹图谱的变化,评价山药饮片辐射灭菌的可行性。方法:采用Diamonsil C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸水溶液,梯度洗脱,流速1.0 ml·min^-1,检测波长258 nm,柱温30℃。分别采用辐照剂量4,6,8,10 kGy对山药饮片粉末进行静态辐照,应用配对t检验对各辐照剂量前后指纹图谱中共有峰的相对保留时间和单位供试品量的峰面积进行统计学分析。结果:通过方法学考察及10批样品的测定,建立了山药饮片的HPLC指纹图谱,共确认了7个共有峰,通过与对照品比对,指认了其中3个色谱峰,分别为尿苷、腺苷与鸟苷,各批样品图谱相似度均大于0.945。经过8,10 kGy剂量辐照后,山药指纹图谱中色谱峰的相对保留时间和单位供试品量的峰面积与辐照前相比差异有统计学意义(P<0.05)。结论:建立的山药指纹图谱方法准确、可靠。山药辐照灭菌时辐照剂量不超过6 kGy为宜。Objective:To establish the HPLC fingerprint of Rhizoma Dioscoreae pieces,and evaluate the radiation sterilization feasibility of Rhizoma Dioscoreae pieces by studying the changes of HPLC fingerprint before and after irradiation by Co-γray.Methods:A Diamonsil C18 column(250 mm×4.6 mm,5μm)was used and the mobile phase consisted of acetonitrile-0.1%phosphoric acid solution with gradient elution at the flow rate of 1.0 ml·min^-1.The detection wavelength was 258 nm and the column temperature was 30℃.Rhizoma Dioscoreae powder was irradiated by 60Co-γray with the dosage of 4,6,8 and 10 kGy,respectively.Paired T test was used to analyze the relative retention time of common peaks and the peak area of each sample before and after each irradiation dose.Results:Through methodological investigation and the determination of 10 batches of samples,the HPLC fingerprint of Rhizoma Dioscoreae pieces was established and 7 common peaks were confirmed.Totally 3 chromatographic peaks were identified by the comparison with the reference substance,namely uridine,adenosine and guanosine.The similarity of each batch of samples was greater than 0.945.After the irradiation with 60Co-γray at the dosage of 8 and 10 kGy,the relative retention time of chromatographic peaks and the peak area per unit of sample quantity changed significantly when compared with those before the irradiation(P<0.05).Conclusion:The established method for HPLC fingerprint of Rhizoma Dioscoreae pieces is accurate and reliable.The radiation dosage of Rhizoma Dioscoreae pieces should not exceed 6 kGy.
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