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本文报告采用国产高效液相色谱仪同时测定血清普鲁卡因酰胺(procaina-mide;PA)及其活性代谢产物N—乙酰普鲁卡因酰胺(N—acetylprocainamide,NAPA)的方法,可于8分钟内完成色谱分析。本法以N—丙酰普鲁卡因酰胺(N-pr-opionyl procainamide NPPA)作为内标,标本在碱性条件下用二氯甲烷提取,在27℃水浴中氮气吹干后,残留物用甲醇重溶进行色谱分析。分析柱为内填国产YWG-CH无定型十八烷基硅烷的150×5mm的不锈钢柱。流动相为乙腈:甲醇:1%冰醋酸(9/13/78,V/V)的混合液,每100ml内加正丁胺30μl,用12.5mol/L NaOH调至ph5.5。在254nm检测器上进行检测。本法PA、NAPA的检出限均为0.5μg/ml,至少80μg/ml以内呈线性,PA及NAPA的变异系数分别为1.93%和3.63%,相对回收率分别为95.2—96.9%和91.6—96.5%。未发现干扰本测定的药物。
This article reports the simultaneous determination of serum procaina-mide (PA) and its active metabolite N-acetylprocainamide (NAPA) using a domestic HPLC, Chromatographic analysis completed within minutes. In this method, N-propionyl procainamide (NPPA) was used as an internal standard. The samples were extracted with dichloromethane under basic conditions. After drying in a water bath at 27 ° C, the residue was washed with Methanol was re-dissolved for chromatographic analysis. The analytical column is a 150 × 5mm stainless steel column packed with a domestic-made YWG-CH amorphous octadecylsilane. The mobile phase consisted of a mixture of acetonitrile: methanol: 1% glacial acetic acid (9/13/78, V / V). Add n-butylamine 30μl to 100ml and adjust to ph5.5 with 12.5mol / L NaOH. Detection was done on a 254 nm detector. The detection limits of PA and NAPA in this method were 0.5μg / ml and linear within at least 80μg / ml. The coefficients of variation of PA and NAPA were 1.93% and 3.63%, respectively. The relative recoveries were 95.2-96.9% and 91.6- 96.5%. No interference with this assay was found.