石斛夜光丸中五味子的质量控制研究  

Qualitycontrol of Schisandraee Chinensis Fructus in Shihu Yeguang pills

作　　者：何颂华 覃丽郦 李丽莉 马双成[2] HE Song-hua;QIN Li-li;LI Li-li;MA Shuang-cheng(Guangxi Institute for Food and Drug Control,NMPA Key Laboratory for Quality Monitoring and Evaluation of Traditional Chinese Medicine,Chinese Material Medica,Nanning 530021,China;National Institutes for Food and Drug Control,Beijing 102629,China)

机构地区：[1]广西食品药品检验所、国家药品监督管理局中药材质量监测与评价重点实验室,南宁530021 [2]中国食品药品检定研究院,北京102629

出　　处：《药物分析杂志》2023年第4期685-692,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立石斛夜光丸中五味子定性鉴别方法和掺伪检查方法,以控制石斛夜光丸中五味子的投料质量。方法:采用薄层色谱法对石斛夜光丸中五味子进行定性鉴别,以环己烷-乙酸乙酯(3∶2)为展开剂,在紫外光灯(254 nm)下检视。采用液相色谱-质谱联用法对安五酯素、五味子醇甲进行测定,计算安五脂素与五味子醇甲的含量比值,如比值>2.0,则存在以南五味子代替五味子投料的情况;色谱条件:采用Agilent Eclipse C18(100 mm×2.1 mm,1.8μm)色谱柱,柱温35℃,以乙腈(A)^(-1)0 mmol·L^(-1)乙酸铵溶液(B)为流动相,梯度洗脱,流速0.25 mL·min^(-1),进样量1μL。结果:对收集的19家企业的91批石斛夜光丸进行了检测,其中1个企业的3个批次样品存在以南五味子代替五味子投料的情况,薄层色谱鉴别方法和液相色谱-质谱联用掺伪检查方法的检测结果一致。结论:本方法准确、可靠,可作为石斛夜光丸中五味子质量控制的检测方法。Objective:To establish the Qualitative identification and adulteration inspection methodsof Schisandrae Chinensis Fructus in Shihu Yeguang pills.Methods:TLC was used for qualitative identification of Schisandrae Chinensis Fructus.Cyclohexane-ethyl acetate(3∶2)was used as developing solvent and the plate was detected under ultraviolet lamp(254 nm).LC-MS was used for the qualification of anwuligan and schizandrin.The content ratio of anwuligan and schizandrin as a threshold could be used to discriminate.If the ratio was above 2.0,the Shihu Yeguang pills were added Schisandrae Sphenanthera Fructus.An Agilent Eclipse C_(18)(100 mm×2.1 mm,1.8μm)column was adopted,and the column temperature was 35℃.Injection volume was 1μL,acetonitrile and 10 mmol·L^(-1)ammonium acetatesolution was used as the mobile phase for gradient elution,and the flow rate was 0.25 mL·min^(-1).Results:91 batches of Shihu Yeguang pills from 19 enterprises were tested,Schisandrae Sphenanthera Fructus was detected from 3 batches of samples.The result of TLC was consistent with the result of LC-MS.3 batches of samples from an enterprise were detected for addition of Schisandrae Sphenanthera Fructus.Conclusion:The method is accurate and reliable,which can be applied to quality control of Schisandrae Chinensis Fructus in Shihu Yeguang pills.

关 键 词：石斛夜光丸 安五脂素 五味子醇甲 南五味子 五味子 薄层色谱法 液相色谱-质谱联用 

分 类 号：R917[医药卫生—药物分析学]