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参归益血合剂质量标准研究

Study on Quality Standard of Shengui Yixue Mixture

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目的 建立参归益血合剂的质量标准.方法 采用薄层色谱(TLC)法对制剂中的虎杖、当归、白芍进行定性鉴别;采用高效液相色谱法测定芍药苷的含量,色谱柱为Hypersil GOLD C18 柱(250 mm×4.6 mm,5 μm),流动相为乙腈-0.1%磷酸水溶液(梯度洗脱),流速为 1.0 mL/min,检测波长为 230 nm,柱温为 30℃,进样量 5 μL.结果 3 种药材TLC图斑点清晰,分离度好,且阴性对照无干扰.芍药苷的质量浓度在 0.00732~0.1464 mg/mL范围内与峰面积线性关系良好(R2=0.9998,n=5);精密度、稳定性、重复性试验结果的RSD均小于 1.0%;平均加样回收率为 101.92%,RSD为 0.66%(n=6).3 批样品中芍药苷含量分别为 0.2640,0.2819,0.2716 mg/mL.结论 本研究中所建方法操作简便、结果准确可靠,可用于参归益血合剂的质量控制.
Objective To establish the quality standard of Shengui Yixue Mixture.Methods Polygoni Cuspidati Rhizoma et Radix,Angelicae Sinensis Radix and Paeoniae Radix Alba in the preparation were qualitatively identified by the thin-layer chromatography(TLC)method.The content of paeoniflorin was determined by the high-performance liquid chromatography(HPLC)method;the chromatographic column was the Hypersil GOLD C18 column(250 mm×4.6 mm,5 μm),the mobile phase was acetonitrile-0.1%phosphoric acid aqueous solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was 230 nm,the column temperature was 30℃,and the injection volume was 5 μL.Results The TLC chromatograms of the three medicinal herbs showed clear characteristic spots,good resolution,and there was no interference from the negative reference.The linear range of paeoniflorin was 0.00732-0.1464 mg/mL(R2=0.9998,n=5).The RSDs of precision,stability and repeatability tests were all lower than 1.0%.The average recovery rate of paeoniflorin was 101.92%with an RSD of 0.66%(n=6).The contents of paeoniflorin in three batches of samples were 0.2640,0.2819,0.2716 mg/mL,respectively.Conclusion The established method is easy,accurate and reliable,which can be used for quality control of Shengui Yixue Mixture.

Shengui Yixue Mixturequality standardTLCHPLCpaeoniflorincontent determination

李小伟、张松、牛倩、吴鸿飞

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安徽省亳州市蒙城县中医院,安徽 亳州 233500

安徽省亳州职业技术学院,安徽 亳州 236800

安徽中医药大学药学院,安徽 合肥 230031

参归益血合剂 质量标准 薄层色谱法 高效液相色谱法 芍药苷 含量测定

安徽省高校自然科学研究项目

KJ2021A1432

2024

中国药业
重庆市食品药品监督管理局

中国药业

CSTPCD
影响因子:1.369
ISSN:1006-4931
年,卷(期):2024.33(16)