摘要
建立了HPLC法测定二丁酰环磷腺苷钙(1)原料药中的有关物质,分别为2'-O-单丁酰环磷腺苷钠(3)、N~6-单丁酰环磷腺苷钠(4)、环磷腺苷(5)。采用ODS Hypersil色谱柱(4.6 mm×200 mm,5μm),以0.1 mol/L磷酸二氢钾溶液和甲醇(体积比600∶400)为流动相,检测波长为273 nm;柱温为30℃;流速为1.0 mL/min。建立了加校正因子的主成分自身对照法测定3种已知杂质,确定了3、4、5相对主成分的校正因子,分别是1.7、0.9、1.4。结果显示,二丁酰环磷腺苷钠(2)和3、4、5分别在0.1~20、4~20、1~20、0.1~2μg/mL内线性关系良好。3、4、5的平均加样回收率(n=2)分别为101.0%、98.5%、99.7%,精密度RSD(n=6)分别为0.1%、0.2%、0.1%,重复性RSD(n=6)分别为1.5%、1.6%、2.5%。3、4、5和1的检测限分别为0.2、0.1、0.1、0.2 ng。该方法专属性好、准确度和灵敏度高,为1的质量研究提供了参考。
An HPLC method was established to determine the related substances in calcium dibutyryladenosine cyclophosphate(1)bulk drug,which were sodium 2'-O-monobutyryladenosine cyclophosphate(3),sodium N°monobutyryladenosine cyclophosphate(4)and adenosine cyclophosphate(5).The ODS Hypersil column(4.6 mm×200 mm,5μm)was used,with 0.1 mol/L potassium dihydrogen phosphate solution-methanol(600:400)as the mobile phase.The detection wavelength was 273 nm,the column temperature was 30 C and the flow rate was 1.0 mL/min.A main component self-compare with correction factor method was established to determine three known impurities,and the correction factors of impurities 3,4,and 5 to the principal component were determined to be 1.7,0.9,and 1.4,respectively.The results showed that it was linear for sodium dibutyryladenosine cyclophosphate(2),3,4,5 in the ranges of 0.1-20,4-20,1-20,0.1-2μg/mL,respectively.The average recoveries(n=2)of 3,4 and 5 were 101.0%,98.5%,and 99.7%,respectively,and the precision RSDs(n=6)were 0.1%,0.2%,and 0.1%,respectively.The repeatability RSDs(n=6)were 1.5%,1.6%,and 2.5%,respectively.The detection limits for 3,4,5,and 1 were 0.2,0.1,0.1,and 0.2 ng,respectively.This method has good specificity,accuracy,and sensitivity,which can provide a reference for quality research of 1.
作者
孙珍
徐明明
严翠霞
郑璐侠
邵泓
SUN Zhen;XU Mingming;YAN Cuixia;ZHENG Luxia;SHAO Hong(NMPA Key Lab.for Quality Control of Therapeutic Monoclonal Antibodies,Shanghai Institute of Food and Drug Control,Shanghai 201203)
出处
《中国医药工业杂志》
EI
CAS
CSCD
2024年第1期101-106,共6页
Chinese Journal of Pharmaceuticals
关键词
二丁酰环磷腺苷钙
HPLC
有关物质
加校正因子的主成分自身对照法
calcium dibutyryladenosine cyclophosphate
HPLC
related substance
main component self-compare with correctionfactormethod
