医药导报2012，Vol.31Issue(2)：199-202,4.DOI:10.3870/yydb.2012.02.027
固相萃取离子色谱法测定反义寡核苷酸药物杂质
Determination of Impurities in the Oligonucleotide by Solid Phase Extraction Ion-chromatography
摘要
Abstract
Objective An solid-phase-extraction ion chromatography was developed for determining three residual impurities such as acetic acid ( MCAA) , dichloroacetic acid ( DCAA) and chloride ion ( Cl- ) in crude oligonucleotide simultaneously. Methods The final optimized conditions for testing were listed as follows by using Ionpac AS 23 (4 mm× 250 mm) analytical column, Ionpac AG23 (4 mmx50 mm) protective column, mobile phase as 0. 8 mmol·L-1 NaHCO3/ 4.5 mmol ·L-1 Na2CO3 and suppressed conductivity detector. Results The standard curve equation of MCAA, DCAA and Cl" were Y= 5.230 7X+0.014 (r = 0.999 7) , Y= 19. 762X-0. 007 2 (r = 0.999 9) and Y=507. 4X-0. 746 2 (r = 0.999 8) , respectively; MCAA,DCAA and Cl" showed a good linearity in 0. 002-0. 400 μg · mL-1 , 0. 000 624-0. 156 μg · mL-1, 0. 002 4-1. 5 mg · mL-1 and detection limits were 0. 02 ,0. 312 ng · mL-1 and 0. 01 μg · mL-1 ,respectively. Conclusion The method is simple,fast,accuracy and can be used for impurities control of crude oligonucleotide.关键词
反义寡核苷酸/离子色谱法/杂质/醋酸/二氯乙酸/氯离子Key words
Antisense oligonucleotides/ Ion-chromatography/Impurities/Acetic acid/Dichloroacetic acid/ Chlorideion分类
医药卫生引用本文复制引用
马金平,仲婕,鲁丹丹,张金钟,施明珠,高婵,朱德领..固相萃取离子色谱法测定反义寡核苷酸药物杂质[J].医药导报,2012,31(2):199-202,4.基金项目
"十二五"国家重大新药创制科技重大专项(2011ZX09102-001-07) （2011ZX09102-001-07）
"十二五"国家重大新药创制科技重大专项(2011ZX09102-009-09) （2011ZX09102-009-09）
