全血中利多卡因的高效液相色谱法测定

DETERMINATION OF LIDOCAINE IN WHOLE BLOOD BY HPLC

本文报道反相高效液相色谱法测定全血中利多卡因浓度的方法。氟安定作为内标,全血经溶血,1N 氢氧化钠1ml 碱化后,用乙醚提取。以Zorbax ODS 为固定相,以CH_3 OH∶H_2O∶(C_2H_5) _3N(100∶45∶0. 2,pH6. 3) 为流动相,检测波长为240nm。用利多卡因为内标的峰高比定量。血中利多卡因最低检出浓度为0. 125ug/ml。线性范围是0. 0025～0. 0750mg/ml(r=0. 9999) 和0. 0250～0. 3000mg/ml(r=0. 9999) 。本法添加利多卡因1. 0、2. 5,8. 0ug 的回收率分别为101. 51±1. 51%、98. 10±2. 05%和±98. 09±3. 63%,天内变异系数分别为1. 49、1. 29和3. 70,天间变异系数为1. 78%。

It is reported here the determination of lidocaine in whole blood by reserved-phase HPLC.Lidocaine and the internal standard,fluazepam is separated wellby Zorbax ODS and CH_3OH:H_2O:(C_2H_5) _3N (100:45:0. 2,pH6. 3) .The eluate ismonitored at UV 240nm.The procedure of sample preparation is described bellow:1ml distilled water was added to 1 ml of whole blood,shake for 30 second.Then 5 μl internal standard (0. 1mg/ml),1 ml 1N Sodium hydroxide and 5 mlether was added.After shaking for 2 minutes,the sample was centrifuged for 6minutes at 3500rpm.The ether part was separated and evaperated to dryness at45℃ under air flow.The residue is solved in 50μl methanol.10 μl preparedmethanol was injected.The limit of lidocaine in whole blood is 0. 125μg/ml.The first linear range is from 0. 0025 to 0. 0750 mg/ml (r=0. 9999) and anotherlinear range is from 0. 0250 to 0. 3060 mg/ml(r=0. 9999) .The recovery by adding 1. 0,2. 5,8. 0 μg lidocaine is 101. 51±1. 51%,98. 10±2. 05%,and 98. 09±3. 63% respec-tively.The coefficient variation within day by adding 1. 0,2. 5,8. 0μg lidocaineis 1. 49%(n=5) ,1. 29%(n=5) ,and 3. 70%(n=6) respectively.And the coefficientvariation day to day by adding 2. 5μg lidocaine is 1. 78%(n=5) .