^(60)Co-γ射线辐照灭菌对幼泻宁颗粒高效液相色谱指纹图谱和活性成分含量的影响  

Effect of^(60)Co-γ-Ray Irradiation Sterilization on HPLC Fingerprint and Active Ingredient Content in Youxiening Granules

作　　者：邬倩 卫蓓蓓 陈维中[1] WU Qian;WEI Beibei;CHEN Weizhong(The 900th Hospital of the Joint Logistics Support Force of the Chinese PLA,Fuzhou,Fujian,China 350000)

机构地区：[1]中国人民解放军联勤保障部队第九○○医院医疗保障中心,福建福州350000

出　　处：《中国药业》2025年第9期80-84,共5页China Pharmaceuticals

摘　　要：目的探讨^(60)Co-γ射线辐照灭菌对幼泻宁颗粒中活性成分含量的影响,以及辐照灭菌前后高效液相色谱指纹图谱的变化。方法采用0,3,6,8 kGy^(60)Co-γ射线对样品进行辐照灭菌,采用高效液相色谱(HPLC)法测定样品中木犀草素、木犀草苷、白术内酯Ⅰ、白术内酯Ⅱ、白术内酯Ⅲ的含量,色谱柱为Agilent Zorbax-C_(18)柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.35%磷酸溶液(梯度洗脱),流速为0.8 mL/min,检测波长为350 nm(0~38 min)和220 nm(38~60 min),柱温为40℃,进样量为10μL。通过中药色谱指纹图谱相似度评价系统(2012版)构建10批样品的HPLC指纹图谱,并评价相似度。结果样品经0,3,6,8 kGy^(60)Co-γ射线辐照后的HPLC指纹图谱中均标定21个共有峰,指认出5号峰为木犀草苷、6号峰为木犀草素、17号峰为白术内酯Ⅲ、18号峰为白术内酯Ⅱ、19号峰为白术内酯Ⅰ,相似度分别为0.9999±0.0001、0.9996±0.0002、0.9687±0.0009、0.8327±0.0015。木犀草素、木犀草苷、白术内酯Ⅰ、白术内酯Ⅱ、白术内酯Ⅲ的进样量分别在0.1001~1.5015μg、0.0535~0.7972μg、0.2026~3.0390μg、0.1338~2.0070μg、0.1612~2.4180μg范围内与峰面积线性关系良好(r≥0.9996,n=6);检测限分别为0.010,0.008,0.020,0.009,0.009μg/mL,定量限分别为0.02,0.01,0.06,0.02,0.04μg/mL;精密度、稳定性、重复性试验结果的RSD均小于2.0%;加样回收率分别为99.36%,98.77%,99.97%,101.04%,99.13%,RSD分别为0.69%,0.74%,0.43%,0.98%,1.24%(n=6)。≤6 kGy^(60)Co-γ射线辐照条件下,样品中上述5种成分的含量均无显著差异(P>0.05)。结论^(60)Co-γ射线辐照灭菌法能较好地控制幼泻宁颗粒的活性成分及HPLC指纹图谱,是一种安全、高效的灭菌方法。Objective To investigate the effect of^(60)Co-γ-ray irradiation sterilization on the content of active ingredients in Youxiening Granules,and the changes in high-performance liquid chromatography(HPLC)fingerprints before and after irradiation sterilization.Methods The samples were irradiated with 0,3,6,and 8 kGy^(60)Co-γrays for sterilization.The contents of luteolin,luteolin-7-glucoside,atractylodesⅠ,atractylodesⅡ,atractylodesⅢin samples were determined by HPLC method,the chromatographic column was Agilent Zorbax-C_(18)column(250 mm×4.6 mm,5µm),the mobile phase was acetonitrile-0.35%phosphoric acid aqueous solution(gradient elution),the flow rate was 0.8 mL/min,the detection wavelengths were 350 nm(0-38 min)and 220 nm(38-60 min),the column temperature was 40℃,and the injection volume was 10µL.The HPLC fingerprints of 10 batches of samples were established and the similarity was evaluated by the Similarity Evaluation System for Chromatographic Fingerprinting of Traditional Chinese Medicine(2021 Version).Results In the HPLC fingerprints of the samples irradiated at the dose of 0,3,6,and 8 kGy^(60)Co-γrays,21 common peaks were identified,peak 5 was identified as verbascoside,peak 6 was identified as verbascoside,peak 17 was identified as atractylodesⅢ,peak 18 was identified as atractylodesⅡ,and peak 19 was identified as atractylodesⅠ,with similarity values of 0.9999±0.0001,0.9996±0.0002,0.9687±0.0009,and 0.8327±0.0015,respectively.The linear ranges of luteolin,luteolin-7-glucoside,atractylodesⅠ,atractylodesⅡ,atractylodesⅢwere 0.1001-1.5015µg,0.0535-0.7972µg,0.2026-3.0390µg,0.1338-2.0070µg,and 0.1612-2.4180µg(r≥0.9996,n=6),respectively.The limits of detection were 0.010,0.008,0.020,0.009,0.009µg/mL,respectively.The limits of quantification were 0.02,0.01,0.06,0.02,0.04µg/mL,respectively.The RSDs of precision,stability,and repeatability test results were all lower than 2.0%.The average recoveries of luteolin,luteolin-7-glucoside,atractylodesⅠ,atractylodesⅡ,atractylodesⅢwer

关 键 词：幼泻宁颗粒 ^(60)Co-γ射线辐照灭菌 高效液相色谱指纹图谱 木犀草素 木犀草苷 白术内酯Ⅰ 白术内酯Ⅱ 白术内酯Ⅲ 质量控制 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学] R286.0