摘要
分别建立了高效液相色谱-蒸发光散射(evaporative light scattering detector,ELSD)和电喷雾检测器(charged aerosol detector,CAD)测定注射用益气复脉(冻干)(Zhusheyong Yiqi Fumai,YQFM)中4种糖含量,并对影响CAD测定方法准确性的因素进行探讨。HPLC-ELSD采用Shodex Asahipak NH2P-50色谱柱,流动相为乙腈-水(75∶25),流速为0.8 mL·min-1,ELSD检测器漂移管温度为80℃;HPLC-CAD采用相同色谱柱,乙腈-水梯度洗脱,流速为0.8 mL·min-1,CAD检测器雾化器温度为45℃,功能参数PF(power function)为1.3。YQFM样品分别经ELSD和CAD检测,显示YQFM由果糖、葡萄糖、蔗糖和麦芽糖等4种糖组成。2种方法线性关系良好,且2种方法测得4种糖的加样回收率及重复性、稳定性皆符合方法学要求。初步得出结论:即ELSD和CAD皆能准确测定YQFM中的4种糖含量。通过该研究首次揭示了CAD的PF对糖测定的准确性有重要影响,是CAD法准确测定的关键参数。同时CAD检测器作为非线性检测器,亦可采用线性回归方式,其结果与对数回归无显著性差异。
Evaporative light scattering detector(ELSD) and charged aerosol detector(CAD) methods were established in this study for the content determination of four kinds of sugars in Zhusheyong Yiqi Fumai(YQFM), and the factors affecting the accuracy of CAD methods were discussed. HPLC-ELSD chromatographic separation was performed on a Shodex Asahipak NH2 P-50 column with acetonitrile-water(75∶25)as the mobile phase, with a flow rate of 0.8 mL·min-1, drift tube temperature of 80 ℃. The analysis by HPLC-CAD was performed on the same column with acetonitrile-water as mobile phase for gradient elution, with a flow rate of 0.8 mL·min-1, a neb temperature of 45 ℃, and power function(PF) of 1.3. The samples of YQFM were detected by ELSD and CAD respectively. It was found that YQFM was composed of fructose, glucose, sucrose and maltose. The linear relationship of the two methods was good, and the recoveries, reproducibility and stability of these four kinds of sugars measured by the two methods satisfied the requirements of methodology. Both CAD and ELSD detectors were accurate and reliable in detecting saccharides components in YQFM. In addition, it was revealed in this study for the first time that the PF parameter of CAD had an important influence on the accuracy of sugar determination and acted as the key parameter of CAD method. It was also found that for CAD, a non-linear detector, there was no significant difference between the results of linear regression and logarithmic regression.
作者
王莹
刘芫汐
岳洪水
许玮仪
曹建明
金红宇
马双成
WANG Ying;LIU Yuan-xi;YUE Hong shui;XU Wei-yi;CAO Jian-ming;JIN Hong-yu;MA Shuang-cheng(National Institutes for Food and Drug Control,Bejing 100050,China;Tianjin Tasly Pride Pharmaceutical Co.,Ltd.,Tianjin 300402,China;Thermo Fisher Scientific,Shanghai 201206,China)
出处
《中国中药杂志》
CAS
CSCD
北大核心
2020年第22期5511-5517,共7页
China Journal of Chinese Materia Medica
基金
天津市科技计划项目(18YFCZZC00430)。
关键词
注射用益气复脉(冻干)
蒸发光散射检测器
电喷雾检测器
功能参数
Zhusheyong Yiqi Fumai
evaporative light scattering detector(ELSD)
charged aerosol detector(CAD)
power function
