连翘苷荧光传感器的构建和应用

以柠檬酸为碳源,三聚氰胺和甲醛为双掺杂剂合成碳量子点,并对合成的量子点进行透射电镜(TEM)、傅里叶变换红外光谱(FTIR)、X射线粉末衍射(XRD)、紫外吸收光谱(UV)和荧光光谱(RF)表征,结果表明该量子点粒径均一,发光稳定,适合用作荧光探针。优化了碳量子点含量、pH、反应时间以及温度等影响因素,结果显示检测波长λmax=425 nm时,连翘苷在0.008~0.030 mg/mL范围内有良好的线性关系,1/△f=0.00005(1/c)+0.0003(R2=0.9948),加标回收率在92.5%~106.3%之间,RSD<5%,且干扰物质、反应时间、温度等因素在一定范围内对实验结果的测定无影响。该方法可用于药剂中连翘苷含量的测定。     

高效液相色谱-质谱法同时测定清热解毒口服液中的5种有效成分

建立了同时测定清热解毒口服液中的绿原酸、栀子苷、黄芩苷、连翘苷和靛玉红5种有效成分的高效液相色谱-电喷雾电离质谱（HPLC-ESI/MS）分析方法。采用Zorbax SB C18色谱柱,以含0.2%甲酸的0.4 mmol/L醋酸钠(A相)、乙腈(B相)为流动相进行梯度洗脱,在ESI正离子模式下,采用选择离子监测方法进行测定,用峰面积进行定量。结果表明,绿原酸、栀子苷、黄芩苷、连翘苷和靛玉红的线性范围分别为0.050～50 mg/L,0.020～20 mg/L,0.005～30 mg/L,0.010～15 mg/L和0.010～10 mg/L;检出限分别为0.010,0.005,0.001,0.002和0.003 mg/L。5种成分的加样回收率为97.0%～101.7%,相对标准偏差小于2.2%。该法快捷、准确、重复性好,可用于清热解毒口服液中的5种有效成分含量的同时测定。     

Determination of baicalin, chlorogenic acid and forsythin in Chinese medicinal preparation by capillary electrophoresis

Summary The determination of baicalin, chlorogenic acid and forsythin in a traditional Chinese medicinal preparation, Shuanghuanglian oral liquid, has been investigated by micellar electrokinetic capillary electrophoresis using borate buffer, SDS and acetonitrile as background electrolyte, 15 kV applied voltage and UV detection, the three active compounds were completely separated within 15 min. The effect of buffer pH, concentration of borate and SDS are discussed. Regression equations reveal linear relationships between the peak-area of each component and content. In addition, the levels of three active compounds in traditional Chinese medicinal preparation, Shuanghuanglian oral liquid, were easily determined with recoveries of 95.20–105.73%.     

激光拉曼光谱法测定不同采收期连翘叶中连翘苷的含量

采用激光拉曼光谱内标法对不同采收期连翘叶中连翘苷的含量进行测定。分别选取连翘苷甲醇溶液的拉曼光谱中连翘苷呋喃环上C-H对称伸缩振动(2844 cm-1处强峰)和溶剂甲醇中CH3-O反对称伸缩振动(2975 cm-1)作为定量峰和内标参比峰。以两拉曼峰峰强的比值组成相对强度,绘制标准曲线,并对线性和加样回收率进行考察。在1.1×10-5mol.L-1~3.5×10-4mol.L-1(5.9 mg.mL-1~189.1 mg.mL-1)范围内,连翘苷的浓度与相对峰强的线性关系良好,r=0.9980,检出限为5.2×10-6mol.L-1.通过精密度、重复性和加样回收率测定,结果证明该法具有良好的精密度、重复性和准确性。对不同采收期的连翘叶样品进行了测定,结果表明该法简便快速、高效灵敏,可用于其含量测定。拉曼光谱内标法用于连翘苷的定量分析具有操作简便和无需添加其它试剂等优点,可以用于药物的含量测定。