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  

Simultaneous Determination of 6 Carbohydrate Related Substances in Glucose by HPLC-ELSD

作　　者：宫兴华 郑磊 李娟[2] GONG Xinghua;ZHENG Lei;LI Juan(Dept.of Pharmacy,Shandong Provincial Third Hospital,Jinan 250031,China;Dept.of Pharmacy,the Second Hospital of Shandong University,Jinan 250033,China)

机构地区：[1]山东省立第三医院药学部,济南250031 [2]山东大学第二医院药学部,济南250033

出　　处：《中国药房》2021年第10期1241-1245,共5页China Pharmacy

基　　金：山东省自然科学基金资助项目(No.ZR2017BH014);山东省重点研发计划(No.2018GSF118010)。

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XBridge Amide,流动相为乙腈-水(75∶25,V/V),流速为0.5 mL/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40 psi,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(12 h)、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、0~1.89 mg/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。OBJECTIVE:To establish the method 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 5.99-59.88,9.90-98.96,9.92-99.19,5.97-59.74,4.03-40.32,5.89-58.89μg/mL(r>0.9990).The quantitation limits were 1.5,1.5,1.5,3.0,3.0 and 3.0μg/mL,respectively.The detection limits were 0.5,0.5,0.5,1.0,1.0,1.0μg/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.

关 键 词：葡萄糖 糖类 有关物质 高效液相色谱-蒸发光散射检测法 

分 类 号：R917[医药卫生—药物分析学]