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目的建立一种准确的测定血浆中甲氧氯普胺含量的气相色谱-质谱(GC-MS)联用方法。方法对萃取溶剂的种类和萃取p H值进行优化。取0.5 ml待测血浆,加入0.01 mol/L盐酸2 ml,加入碳酸铵0.5 g,振荡2 min,加入0.1 mol/L Na OH溶液调节p H值至9.0,加入二氯甲烷-乙酸乙酯(9∶1,V/V)混合溶液2 ml,涡旋提取3 min,3 500 r/min离心,取有机层,氮气吹干,用50μl乙酸乙酯溶解残渣,取1μl进样分析。结果血浆中甲氧氯普胺浓度在0.1μg/ml~20.0μg/ml线性关系良好,回归方程为y=5.535 3x+0.463 2,r=0.999 3,检测限为0.01μg/ml,日内精密度为3.39%~4.24%,日间精密度为4.01%~5.11%,回收率为90.73%~105.22%。结论本方法灵敏度高,重现性好,可在法医鉴定和临床血药浓度监测过程中准确定量。
Objective To establish an accurate method for the determination of metoclopramide in plasma by gas chromatography-mass spectrometry (GC-MS). Methods The extraction solvent type and extraction p H value were optimized. Take 0.5 ml of plasma to be tested, add 2 ml of 0.01 mol / L hydrochloric acid, add 0.5 g of ammonium carbonate and shake for 2 min, adjust p H value to 9.0 by adding 0.1 mol / L NaOH solution, add methylene chloride-ethyl acetate Vortexed for 3 min and centrifuged at 3 500 r / min. The organic layer was dried under nitrogen and dissolved in 50 μl of ethyl acetate. 1 μl of the sample was analyzed by injections. Results The linearity of metoclopramide in plasma ranged from 0.1μg / ml to 20.0μg / ml. The regression equation was y = 5.535 3x + 0.463 2, r = 0.999 3, and the detection limit was 0.01μg / ml. The intra- The accuracy was 4.01% -5.11% during the day, and the recoveries ranged from 90.73% to 105.22%. Conclusion The method has high sensitivity and good reproducibility, and can be accurately quantified in the forensic identification and clinical blood concentration monitoring.