首页|DTDPA-OPA联合柱前衍生化HPLC测定普卡那肽原料药中的氨基酸比值

DTDPA-OPA联合柱前衍生化HPLC测定普卡那肽原料药中的氨基酸比值

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采用HPLC法,以二硫代二丙酸(DTDPA)和邻苯二甲醛(OPA)联合作为柱前衍生化试剂,建立了普卡那肽原料药中氨基酸比值的测定方法.结果显示,普卡那肽中各氨基酸的定量限为0.006 9~0.012 7 μmol/mL,检测限为0.003 5~0.006 3 μmol/mL,在定量限至测定浓度的200%范围内,线性关系良好(r≥0.999 6);溶液稳定性RSD(n=9)≤4.058%;氨基酸比值的精密度RSD(n=12)≤2.41%;平均回收率(n=9)在97.32%~101.96%,RSD≤1.22%;检测条件发生微小变化时,氨基酸比值的RSD(n=16)≤1.61%.该法专属性强、准确、高效,可用于普卡那肽氨基酸比值的测定.
Determination of Amino Acid Ratios in Plecanatide by DTDPA-OPA Combined with Pre-column Derivatization HPLC
An pre-column derivatization HPLC method with dithiodipropionic acid(DTDPA)and o-phthalaldehyde(OPA)was established to determine the amino acid ratios in plecanatide.The results showed that the quantitative limits were 0.006 9-0.012 7 μmol/mL,the detection limits were 0.003 5-0.006 3 μmol/mL.The linearity and solution stability of all amino acids were good with minimum r of 0.999 6 and the maximum RSD(n=9)of 4.058%.The precision was good with the maximum RSD(n=12)of 2.41%.The mean recoveries(n=9)were 97.32%-101.96%,the maximum RSD was 1.22%.In case of detection parameters slight change,the durability was good with the maximum RSD(n=16)of 1.61%.The established method is specific,accurate and efficient,which can be used for determination of the amino acid ratios of plecanatide.

plecanatideamino acid ratiopre-column derivatizationHPLC

潘静、杨欣茹、李铁健、韩忠丽、张贵民

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鲁南制药集团股份有限公司,国家手性制药工程技术研究中心,山东临沂 273400

普卡那肽 氨基酸比值 柱前衍生化 HPLC

山东省重大科技创新工程项目

2019JZZY010516

2024

中国医药工业杂志
上海医药工业研究院,中国化学制药工业协会

中国医药工业杂志

CSTPCD
影响因子:0.487
ISSN:1001-8255
年,卷(期):2024.55(8)