固相萃取-LC-MS/MS法测定双室中性4.25%腹膜透析液中1,6-己二胺的含量  

Determination of 1,6-Diaminohexane in Two-compartment Neutral 4.25%Peritoneal Dialysis Solution by Solid Phase Extraction-LC-MS/MS

作　　者：吴莹[1] 张静[1] 翟小语 杨敏[1] 张毅兰[1] WU Ying;ZHANG Jing;ZHAI Xiaoyu;YANG Min;ZHANG Yilan(NMPA Key Lab.for Compatibility Studies of Pharmaceutical Products and Packaging Materials,CFDA Research and Inspection Center of Pharmaceutical Packaging Materials,Shanghai Institute of Pharmaceutical Industry,China State Institute of Pharmaceutical Industry,Shanghai 201203)

机构地区：[1]中国医药工业研究总院上海医药工业研究院,国家食品药品监督管理局药品包装材料科研检测中心,国家药品监督管理局药包材与药物相容性研究重点实验室,上海201203

出　　处：《中国医药工业杂志》2021年第8期1087-1092,1096,共7页Chinese Journal of Pharmaceuticals

摘　　要：建立了双室中性4.25%腹膜透析液中1,6-己二胺(1)的固相萃取-LC-MS/MS含量测定方法。双室中性4.25%腹膜透析液中的1经Waters Oasis?MCX固相萃取小柱富集纯化,采用Shim-packScepterPFPP色谱柱(4.6mm×250mm,5μm),以0.1%甲酸溶液∶甲醇(55∶45)为流动相,等度洗脱,流速为1.0ml/min。以1,4-丁二胺为内标,采用电喷雾电离源正离子模式、多反应监测进行定量分析。结果表明,1在3~1000 ng/ml内线性关系良好(r=0.9993),平均回收率(n=3)为97.8%~108.0%,RSD≤6.29%。本方法专属性强、准确性好、灵敏度高,适用于痕量1的测定。A solid phase extraction-LC-MS/MS method for the determination of 1,6-diaminohexane(1)in two-compartment neutral 4.25%peritoneal dialysis solution was established.After concentrated and cleaned by Oasis?MCX solid phase extraction column,samples were separated with a Shim-pack Scepter PFPP column(4.6 mm×250 mm,5μm)at the flow rate of 1.0 ml/min by isocratic elution using 0.1%formic acid and methanol(55∶45)as the mobile phase.1,4-Butanediamine was chosen as the internal standard,and the positive ion mode of electrospray ionization source and multiple reaction monitoring were used for quantitative analysis.The results showed that it was linear for 1 in the range of 3-1000 ng/ml(r=0.9993).The average recoveries(n=3)were 97.8%-108.0%,and the RSDs were less than 6.29%.The established method has strong specificity,good accuracy and high sensitivity,which is suitable for the trace determination of 1.

关 键 词：双室中性4.25%腹膜透析液 1 6-己二胺 固相萃取 LC-MS/MS 

分 类 号：R914.1[医药卫生—药物化学]