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出 处:《中南药学》2012年第1期62-66,共5页Central South Pharmacy
基 金:国家自然科学基金重大研究计划课题(No.90612002)
摘 要:目的建立双黄连胶囊(Shuanghuanglian Jiaonang,SHLJN)双波长高效毛细管电泳指纹图谱(DW-CEFP)。方法用三角形和四面体优化法优化出以50mmol.L-1硼砂(含20mmol.L-1β-环湖精和5%乙腈,磷酸调pH 7.55)为背景电解质(BGE),采用未涂层石英毛细管(75cm×75μm,有效分离长度57cm),以色谱指纹图分离量指数(RF)为目标函数优化试验条件,运行电压12kV,检测波长203nm和256nm。用均值法整合双波长谱的宏定性宏定量信息,用一级系统指纹定量法评价SHLJN质量。结果以连翘苷(FST)为参照物峰,在203nm和256nm下检测,分别确定16和11个共有指纹峰,建立了DW-CEFP。用均值法整合后进行评价出S9样品质量极好,S2、S3、S4和S6样品质量很好,S1、S7、S10和S11样品质量好,S5、S8和S12样品质量良好。结论基于双波长谱的一级系统指纹定量法对SHLJN整体定性定量分析具有信息全面、准确可靠的特点,为其质量控制提供一种新参考。Objective To establish dual wavelength capillary electrophoresis fingerprints(DW-CEFP) for Shuanghuanglian Jiaonang(SHLJN). Methods The 75 cm×75 μm(the effective length of 57 cm) uncoated fused silica capillary column was used.The triangle and tetrahedron optimization method was employed to select the background electrolyte of 50 mmol·L-1 sodium borate,containing 20 mmol·L-1 β-cyclodextyin and 5% acetonitrile(pH adjusted to 7.55 with phosphoric acid),and the running voltage was 12 kV,in which the detection wavelength was 203 nm and 256 nm.At the same time the chromatographic fingerprint resolution index was applied to optimize the CEFP conditions.The first systematically quantified fingerprint method(FSQFM) was used to evaluate SHLJN quality.The average method was used to integrate different chemical qualitative and quantitative information from the DW-CEFPs. Results The DW-CEFPs were developed,in which 16 and 11 co-possessing peaks were marked under detection wavelength of 203 nm and 256 nm respectively with forsythin peak as the referential peak.The identification results were obtained by the FSQFM which indicated that the quality of S9 was the best,that of S2,S3,S4 and S6 was better,that of S1,S7,S10 and S11 was good,and that of S5,S8 and S12 was acceptable after integration with average method. Conclusion The FSQFM based on DW-CEFP shows good overall qualitative and quantitative identification of SHLJN.The method can serve as a reference to identify and control the quality of SHLJN.
关 键 词:双黄连胶囊 双波长毛细管电泳指纹图谱 色谱指纹图分离量指数 一级系统指纹定量法
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