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分析化学  2015 

液相色谱-电感耦合等离子质谱和电喷雾电离质谱研究乙二胺二氯合钯与鸟嘌呤脱氧核糖核苷酸反应产物

DOI: 10.11895/j.issn.0253-3820.140692, PP. 193-198

Keywords: 电感耦合等离子体质谱,液相色谱,鸟嘌呤脱氧核糖核苷酸,钯化合物

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Abstract:

建立了基于HPLC-ICP-MS分离乙二胺二氯合钯[Pd(en)Cl2]与鸟嘌呤脱氧核糖核苷酸5'-dGMP反应产物的方法.方法得到两种能够随色谱流出的产物,产物在25mmol/L磷酸盐缓冲液(pH8.0)作为流动相时,得到的分离峰型良好.主产物保留时间为2.8min,另一产物保留时间为3.2min.主产物经富集后由ESI-MS(MS/MS)鉴定得到m/z为510,511,512,514和516的[M+1]+分子离子峰且丰度比与Pd同位素元素一致,再通过碎片推断结构为[Pd(en)(N1-5'-dGMP)],另一种产物经HPLC-DAD解析发现紫外吸收光谱与[Pd(en)(N1-5'-dGMP)]完全相同,HPLC-ICP-MS发现产物含Pd量也与[Pd(en)(N1-5'-dGMP)]相同,结合文献推断另一产物为[Pd(en)(N1-5'-dGMP)]的多聚物.研究表明,[Pd(en)(N1-5'-dGMP)]易在酸性条件下生成,其多聚物易在碱性条件下生成,在反应体系pH=6.0时,[Pd(en)(N1-5'-dGMP)]在12h内生成且稳定存在.HPLC-ICP-MS图谱显示随着反应pH的增加两种产物的总量逐步减少.

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