HPLC-ELSD法同时测定葡萄糖原料药中6种糖类有关物质的含量
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篇名: HPLC-ELSD法同时测定葡萄糖原料药中6种糖类有关物质的含量
TITLE: Simultaneous Determination of 6 Carbohydrate Related Substances in Glucose by HPLC-ELSD
摘要: 目的:建立同时测定葡萄糖原料药中果糖、麦芽糖、异麦芽糖、麦芽三糖、麦芽四糖、麦芽五糖等6种糖类有关物质的方法。方法:采用高效液相色谱-蒸发光散射检测法。色谱柱为XBridgeAmide,流动相为乙腈-水(75∶25,V/V),流速为0.5mL/min,柱温为30℃,进样量为10μL;检测器为蒸发光散射检测器,载气为氮气,气体压力为40psi,蒸发温度为80℃,漂移管温度为80℃,增益为100。结果:上述6种糖类有关物质检测质量浓度的线性范围分别为5.99~59.88、9.90~98.96、9.92~99.19、5.97~59.74、4.03~40.32、5.89~58.89μg/mL(r>0.9990);定量限分别为1.5、1.5、1.5、3.0、3.0、3.0μg/mL,检测限分别为0.5、0.5、0.5、1.0、1.0、1.0μg/mL;精密度、稳定性(12h)、重复性试验的RSD均小于2.0%;平均加样回收率分别为95.87%~98.59%(RSD=1.04%,n=9)、95.66%~99.84%(RSD=1.20%,n=9)、96.11%~98.97%(RSD=1.04%,n=9)、95.06%~99.11%(RSD=1.25%,n=9)、95.69%~98.22%(RSD=0.83%,n=9)、95.34%~98.56%(RSD=1.01%,n=9)。9批葡萄糖原料药中上述6种糖类有关物质含量分别为1.26~2.22、2.55~3.36、2.37~3.37、1.28~2.01、0~2.11、0~1.89mg/g。结论:所建方法准确性好、灵敏度高,可用于葡萄糖中糖类有关物质的检测。
ABSTRACT: OBJECTIVE:To establish the m ethod for the simultaneous determination of 6 carbohydrate related substances in glucose as fructose ,maltose,isomaltose,maltotriose,maltotetraose and maltopentaose. METHODS :HPLC-ELSD was adopted. The determine was performed on XBridge Amide column with mobile phase consisted of acetonitrile-water (75∶25,V/V)at a flow rate of 0.5 mL/min. The column temperature was set at 30 ℃,and the sample size was 10 L. The detector was evaporative light scattering detector ,the carrier gas was nitrogen ,the gas pressure was 40 psi,the evaporation temperature was 80 ℃,the drift tube temperature was 80 ℃,and the gain was 100. RESULTS :The linear range of 6 carbohydrate related substances were 5.99-59.88, 9.90-98.96,9.92-99.19,5.97-59.74,4.03-40.32,5.89-58.89 μg/mL(r>0.999 0). The quantitation limits were 1.5,1.5,1.5,3.0, 3.0 and 3.0 μg/mL,respectively. The detection limits were 0.5,0.5,0.5,1.0,1.0,1.0 μg/mL,respectively. RSDs of precision , stability(12 h)and reproducibility tests were all lower than 2.0%. The average recoveries were 95.87%-98.59%(RSD=1.04%,n= 9),95.66%-99.84%(RSD=1.20%,n=9),96.11%-98.97%(RSD=1.04%,n=9),95.06%-99.11%(RSD=1.25%,n=9), 95.69%-98.22%(RSD=0.83%,n=9),95.34%-98.56%(RSD=1.01%,n=9). The contents of 6 carbohydrate related substances in 9 batches of glucose were 1.26-2.22,2.55-3.36,2.37-3.37,1.28-2.01,0-2.11 and 0-1.89 mg/g,respectively. CONCLUSIONS : Established method is accurate and sensitive ,and can be used for the detection of carbohydrate related substances in glucose.
期刊: 2021年第32卷第08期
作者: 宫兴华,郑磊,李娟
AUTHORS: GONG Xinghua ,ZHENG Lei,LI Juan
关键字: 葡萄糖;糖类;有关物质;高效液相色谱-蒸发光散射检测法
KEYWORDS: Glucose;Carbohydrate;Related substance ;HPLC-ELSD
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