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目的:建立测定胎盘灌流液中安替比林浓度的方法。方法:样品采用液-液萃取预处理后,以高效液相色谱法测定。色谱柱为WatersSymmetryC18,流动相为甲醇∶0.05mol·L-1磷酸氢二钠缓冲液(pH=6.5)=70∶30,内标为非那西丁,流速为1mL·min-1,紫外检测波长为254nm。结果:安替比林检测浓度在1.095~20mg·L-1范围内线性关系良好(r=0.9996);低、中、高3种浓度质控样品的日内RSD分别为5.03%、1.49%、1.53%,日间RSD分别为2.99%、1.01%、0.75%;平均方法回收率为97.19%~103.11%。结论:本方法简便可靠、专属性好、精密度高,可用于胎盘灌流液中安替比林浓度的测定。
Objective: To establish a method for determination of antipyrine concentration in placental perfusate. Methods: Samples were pre-treated with liquid-liquid extraction and determined by high performance liquid chromatography. The chromatographic column was Waters Symmetry C18 with a mobile phase of methanol: 0.05 mol·L -1 disodium hydrogen phosphate buffer (pH = 6.5) = 70:30, the internal standard was phenacetin, the flow rate was 1 mL · min -1, UV detection The wavelength is 254 nm. Results: The linearity of the concentration of antipyrine in the range of 1.095 ~ 20mg · L-1 was good (r = 0.9996). The RSD of low, middle and high quality control samples were 5.03%, 1.49% and 1.53 %, Daytime RSD were 2.99%, 1.01% and 0.75%, respectively. The average recovery was 97.19% ~ 103.11%. Conclusion: This method is simple and reliable, good specificity, high precision, and can be used for determination of concentration of antipyrine in placental perfusate.