联用反相高效液相色谱法和紫外线检测器测定银翘解毒颗粒中绿原酸与连翘苷含量的准确性分析

目的 :探讨联合使用反相高效液相色谱法和紫外线检测器测定银翘解毒颗粒中绿原酸与连翘苷含量的准确性。方法 :用反相高效液相色谱法测定银翘解毒颗粒中绿原酸与连翘苷含量使用的色谱柱为Diamonsil C18柱(250 nm×4.6 mm,5μm),将乙腈-0.4%磷酸水(比例为:20:80)作为流动相,其检测波长为:280nm,其流速为:1.0m L/min。用紫外线检测器测定银翘解毒颗粒中绿原酸与连翘苷含量使用的方法为外标法。结果 :经检测发现,银翘解毒颗粒中绿原酸的线性回归方程为:Y=51649X-614.31,其在103.1ng-2062ng中呈现良好的线性关系(r=0.9995)。银翘解毒颗粒中连翘苷的线性回归方程为:Y=467.01X-58.43,其在18.2ng-364ng中呈现良好的线性关系(r=0.9991)。绿原酸和连翘苷的加样回收率分别为99.93%和99.82%,其RSD分别为1.32%和1.23%。3批次银翘解毒颗粒中绿原酸的平均含量分别为1.02 mg/g、0.97 mg/g、1.14 mg/g,它们中连翘苷的平均含量为0.186mg/g、0.173 mg/g、0.195 mg/g。结论:联合使用反相高效液相色谱法和紫外线检测器测定银翘解毒颗粒中绿原酸与连翘苷含量的准确性很高。此检测方法可作为药学研究机构测定银翘解毒颗粒中绿原酸与连翘苷含量的首选方法。

毛细管电泳紫外法检测重度创伤患者血清谷氨酰胺含量的实验研究

目的探讨重度创伤患者血清中谷氨酰胺(glutamine,Gln)含量准确、简便、快速的检测方法。方法选择我院重度创伤10例(创伤组),分别在术前1 d及术后5、10 d采集静脉血制备血清。选择同期健康体检10例为对照组,同法制备血清。以四硼酸钠(20 mmol/L,pH 9.33)、十二烷基硫酸钠(166 mmol/L)和乙腈按10∶10∶3配置缓冲液,异硫氰酸苯酯为衍生剂,在电压15 kV、紫外吸收波长254 nm下用直径75μm、长58 cm的石英毛细管检测两组血清Gln含量。结果 Gln浓度在0.03～2.00 mmol/L范围内线性关系良好,相关系数为0.9901;精密度为3.14%,平均回收率为92.99%～110.28%;最低检测限浓度为0.01 mmol/L。对照组Gln含量0.79 mmol/L,创伤组术后5 d时Gln出现相对最低点,且术前1 d及术后5、10 d血清Gln浓度均低于对照组,差异有统计学意义(P<0.05)。结论该毛细管电泳紫外法快速、准确而简便,灵敏度高,重复性好,能有效分离检测重度创伤患者血清中Gln含量。

Determination of 5-Fluorouracil in Human Plasma by High-Performance Liquid Chromatography (HPLC)

5-Fluorouracil (5-FU) has a broad spectrum of anti-tumor activity, widely applied to the treatment of cancers. However, it is necessary to determine the plasma concentration of 5-FU in clinical practice due to its narrow therapeutic index. Therefore, a simple, economic and sensitive high-performance liquid chromatography (HPLC) method was developed and validated for the determination of 5-FU in human plasma. Ethyl acetate was chosen as extraction reagent. Chromatographic separation was performed on a Diamonsil C18 column (250 mm × 4.6 mm i.d., 5 μm) with the mobile phase consisting of methanol and 20 mmol/L ammonium formate using a linear gradient elution at a flow rate of 0.8 mL/min. 5-FU and 5-bromouracil (5-BU) were detected by UV detector at 265 nm. The calibration curve was linear over the concentration range of 5—500 ng/mL and the correlation coefficient was not less than 0.992 6 for all calibration curves. The intra- and inter-day precisions were less than 10.5% and 4.3%, respectively, and the accuracy was within ±3.7%. The recovery at all concentration levels was 80.1±8.6%. 5-FU was stable under possible conditions of storing and handling. This method is proved applicable to therapeutic drug monitoring and pharmacokinetic studies of 5-FU in human.

Organic photodetectors based on transparent electrodes for application in ultraviolet light detection

A high performance heterojunction organic ultraviolet photodetector based on NPB and Bphen has been fabricated. A trans- parent conducting polymer PEDOT：PSS coated quartz substrate instead of ITO coated glass substrate as anode is propitious to detect shorter wavelength ultraviolet light. As a result, the device shows a low dark current density, a high responsivity of 502 mA/W and a detectivity of 2.67x1012 cm Hz1/Zfw which is illuminated by a 220 nm ultraviolet light with an intensity of 1.6 mW/cm2. Moreover, the performance of the PEDOT：PSS transparent electrode device is better than the semi-transparent A1 electrode device electrode because of the higher transmittance and electrode properties.