目的 我国糖肽类药物国家标准采用比色法测定多糖含量,游离单糖或二糖会影响含量测定结果,本实验建立了糖肽类药物中游离糖含量测定方法。方法 固相萃取小柱去除样品基体,高效阴离子交换-脉冲安培检测法,CarboPacPA20阴离子交换柱,200 mmol·L-1氢氧化钠溶液和1 mol·L-1醋酸钠溶液梯度洗脱,脉冲安培检测器,金工作电极,Ag/AgCl参比电极,四电位糖检测波形。结果 测定薄芝糖肽、甘露聚糖肽、云芝胞内糖肽原料及制剂20批样品,结果8批样品中检出较高含量游离单糖,包括葡萄糖、蔗糖、甘露糖和果糖。与其他糖检测方法相比,该方法有专属、灵敏、快速、应用范围广等特点。结论 该方法适用于各种糖类化合物的分析,有良好的应用和发展前景;我国糖肽类药物标准中含量测定方法亟待改进。
Abstract
OBJECTIVE To establish a new determination method for free monosaccharides or disaccharides in glycopeptide drugs to eliminate their influence on polysaccharide content assay by colorimetric method adopted by the current national specifications. METHODS Solid phase extraction column was used for matrix elimination. A high performance anion exchange chromatograghy (HPAEC) in conjunction with pulsed amperometric detector (PAD) was performed on a CarboPacPA20,using 200 mmol·L-1 sodium hydroxide solution and 1 mol·L-1 sodium acetate solution as mobile phase. RESULTS Twenty batches of raw materials and preparations of Bozhi glycopeptides, mannatide and polystictus glycopeptide were tested. Free monosaccharides of high content were detected in eight batches of samples, including glucose, sucrose, mannose, and fructose. CONCLUSION The HPAEC-PAD method is specific, sensitive, rapid and applicable widely, compared with other methods of saccharide detection, thus has good prospect of application and development. The assay methods in the current national specifications of glycopeptides drugs need to be improved.
关键词
阴离子交换 /
脉冲安培法 /
糖肽 /
糖含量 /
薄芝糖肽 /
甘露聚糖肽 /
云芝胞内糖肽
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Key words
anion exchange chromatograghy /
pulsed amperometric detection /
glycopeptide /
content /
bozhi glycopeptide /
mannatide /
polystictus glycopeptide
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中图分类号：
R917
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参考文献
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