UPLC-ELSD法快速测定生脉注射液中果糖、葡萄糖、蔗糖、麦芽糖含量
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摘要
目的:建立生脉注射液中主要单糖和双糖含量的快速测定方法。方法:采用超高效液相色谱结合蒸发光散射检测器(UPLC-ELSD)同时测定果糖、葡萄糖、蔗糖、麦芽糖含量。样品经ACQUITY UPLC BEH Amide(2.1 mm×150 mm,1.7μm)色谱柱分离,柱温35℃。流动相为乙腈(含0.2%三乙胺)-水(75∶25),流速0.2 mL·min~(-1)。ELSD检测器漂移管温度55℃,氮气压力40.0 psi。结果:4个成分在各自范围内线性关系良好。果糖、葡萄糖、蔗糖、麦芽糖的平均回收率分别为101.6%、99.1%、99.6%、97.9%。生脉注射液中果糖含量最高,3个生产企业的7批样品糖类成分含量差异较大。结论:该方法简便、快速、灵敏、准确,可为中药注射剂的质量控制和物质基础研究提供参考。
Objective: To establish a rapid determination method of the main monosaccharides and disaccharides in Shengmai Injection. Methods: Fructose, glucose, sucrose and maltose were determined simultaneously by ultra performance liquid chromatography(UPLC) method combined with evaporative light scattering detector(ELSD). Separation was performed on an ACQUITY UPLC BEH Amide(2.1 mm×150 mm, 1.7 μm) column and the column temperature was 35 ℃. The mobile phase consisted of acetonitrile(containing 0.2% triethylamine)-water(75∶25) at a flow rate of 0.2 mL·min~(-1). The temperature for the evaporator tube of ELSD was maintained at 55 ℃ and the gas pressure for nitrogen was 40.0 psi. Results: The calibration curves of the 4 components showed good linearity within their test ranges. The average recoveries for fructose, glucose, sucrose and maltose were 101.6%, 99.1%, 99.6% and 97.9%, respectively. The highest content of sugar in Shengmai Injection was fructose and there was a great variation among contents of sugars in 7 batches of samples from 3 manufactures. Conclusion: The established method was simple, rapid, sensitive and accurate, and could provide references for quality control and substance basis investigation of Traditional Chinese Medicine(TCM) injections.
Objective: To establish a rapid determination method of the main monosaccharides and disaccharides in Shengmai Injection. Methods: Fructose, glucose, sucrose and maltose were determined simultaneously by ultra performance liquid chromatography(UPLC) method combined with evaporative light scattering detector(ELSD). Separation was performed on an ACQUITY UPLC BEH Amide(2.1 mm×150 mm, 1.7 μm) column and the column temperature was 35 ℃. The mobile phase consisted of acetonitrile(containing 0.2% triethylamine)-water(75∶25) at a flow rate of 0.2 mL·min~(-1). The temperature for the evaporator tube of ELSD was maintained at 55 ℃ and the gas pressure for nitrogen was 40.0 psi. Results: The calibration curves of the 4 components showed good linearity within their test ranges. The average recoveries for fructose, glucose, sucrose and maltose were 101.6%, 99.1%, 99.6% and 97.9%, respectively. The highest content of sugar in Shengmai Injection was fructose and there was a great variation among contents of sugars in 7 batches of samples from 3 manufactures. Conclusion: The established method was simple, rapid, sensitive and accurate, and could provide references for quality control and substance basis investigation of Traditional Chinese Medicine(TCM) injections.
引文
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[9]巴晓雨,郝福,张纲,等.HPLC-ELSD法同时测定黄芪注射液中单糖和蔗糖含量[J].亚太传统医药,2017,13(10):25-27.
[10]张利沙,孙玮玮,徐自慧.复方南板蓝根颗粒中多糖的含量测定及单糖组成分析[J].药物分析杂志,2017,37(10):1845-1850.
[11]于雷,李晓坤,张华锋,等.RP-HPLC-RID法同时测定怀地黄中单糖、低聚糖的含量[J].药物分析杂志,2013,33(6):977-982.
[12]张璐,张永丽,姜伟.HPLC-RID法测定天麻蜜环菌片中的D-无水葡萄糖含量[J].江西中医药大学学报,2016,28(6):62-63.
[13]杨成聪,凌霞,胡伟伟,等.高效液相-示差折光法测定米酒中3种糖的含量[J].食品研究与开发,2017,38(21):135-141.
[14]聂黎行,戴忠,林瑞超,等.UPLC法测定愈风宁心滴丸中葛根素的含量[J].中国药事,2013,27(10):1075-1076.
[15]聂黎行,何雨晴,戴忠,等.藿香正气水快速质量评价(Ⅰ)-化学计量学辅助的UPLC指纹图谱研究[J].中国药学杂志,2017,52(20):1862-1866.
[16]聂黎行,何雨晴,于建东,等.藿香正气水快速质量评价(Ⅱ)-超高效液相色谱波长切换法同时测定7个成分的含量[J].中国药学杂志,2017,52(24):2192-2195.
[2]旷湘楠,朱娜,刘时乔.麦冬化学成分研究[J].中国药业,2018,27(2):19-22.
[3]张璐欣,周学谦,李德坤,等.麦冬提取工艺多糖变化规律研究[J].中国现代中药,2017,19(7):1007-1011.
[4]王敏,刘永利,段吉平,等.红参药材与饮片质量评价研究[J].中国药事,2017,31(6):647-652.
[5]陈佳,刘永利,崔志海,等.红参中总还原糖含量测定及限度值拟定[J].中药材,2016,39(10):2426-2429.
[6]凌益平,徐兵勇,刘武,等.HPLC-ELSD测定红参、麦冬及其制剂中糖的含量[J].中国现代应用药学,2014,31(11):1395-1399.
[7]董晓旭,付京,倪健.中药注射剂安全性再评价研究概述[J].山东中医药大学学报,2014,38(4):406-408.
[8]曹树萍,聂黎行,刘丽娜,等.HPLC-ELSD及GC-MS法分析参麦注射液及中间体糖类成分[J].药物分析杂志,2014,34(10):1741-1745.
[9]巴晓雨,郝福,张纲,等.HPLC-ELSD法同时测定黄芪注射液中单糖和蔗糖含量[J].亚太传统医药,2017,13(10):25-27.
[10]张利沙,孙玮玮,徐自慧.复方南板蓝根颗粒中多糖的含量测定及单糖组成分析[J].药物分析杂志,2017,37(10):1845-1850.
[11]于雷,李晓坤,张华锋,等.RP-HPLC-RID法同时测定怀地黄中单糖、低聚糖的含量[J].药物分析杂志,2013,33(6):977-982.
[12]张璐,张永丽,姜伟.HPLC-RID法测定天麻蜜环菌片中的D-无水葡萄糖含量[J].江西中医药大学学报,2016,28(6):62-63.
[13]杨成聪,凌霞,胡伟伟,等.高效液相-示差折光法测定米酒中3种糖的含量[J].食品研究与开发,2017,38(21):135-141.
[14]聂黎行,戴忠,林瑞超,等.UPLC法测定愈风宁心滴丸中葛根素的含量[J].中国药事,2013,27(10):1075-1076.
[15]聂黎行,何雨晴,戴忠,等.藿香正气水快速质量评价(Ⅰ)-化学计量学辅助的UPLC指纹图谱研究[J].中国药学杂志,2017,52(20):1862-1866.
[16]聂黎行,何雨晴,于建东,等.藿香正气水快速质量评价(Ⅱ)-超高效液相色谱波长切换法同时测定7个成分的含量[J].中国药学杂志,2017,52(24):2192-2195.