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目的建立测定人血浆中3种大环内酯类抗菌药物(红霉素、地红霉素、螺旋霉素Ⅰ)及其代谢物(脱水红霉素、红霉素A烯醇醚、红霉胺、新螺旋霉素Ⅰ)的分析方法。方法用乙腈溶液提取,Qu ECHERS方法净化,采用无水硫酸镁和无水乙酸钠沉淀蛋白和盐析分层,无水硫酸镁和石墨碳烯净化,上清液氮气吹干后甲醇复溶待测,用Eclipse Plus C18色谱柱分离,电喷雾正离子模式,多反应离子监测扫描,内标法定量。结果 3种大环内酯类抗菌药物及其代谢物浓度在4~900 ng·mL~(-1)内的线性关系良好(r>0.999),定量限<10 ng·mL~(-1);在3个添加水平下,3种大环内酯类抗菌药物及其代谢物的提取回收率可达81.45%~96.82%,日内精密度<5.00%,日间精密度<10.00%。结论 Qu ECHERS-液相色谱串联三重四级杆质谱测定血浆中3种大环内酯类抗菌药物及其代谢物的分析方法简单,快速,灵敏,特异性强,适用于血浆中大环内酯类抗菌药物及其代谢物的测定。
Objective To establish a method for the determination of three macrolide antibiotics (erythromycin, erythromycin, spiramycin Ⅰ) and their metabolites (erythromycin, erythromycin A enol ether, Amine, Spiramycin I). Methods The samples were extracted with acetonitrile, purified by Qu ECHERS method, precipitated by anhydrous magnesium sulfate and anhydrous sodium acetate, salted-separated and purified by anhydrous magnesium sulfate and carbene. The supernatant was nitrogen-dried and the methanol was reconstituted Measured with Eclipse Plus C18 column separation, electrospray positive ion mode, multi-reactive ion monitoring scan, internal standard method. Results The linear relationship between the concentrations of 3 macrolide antibiotics and their metabolites was in the range of 4 ~ 900 ng · mL -1 (r> 0.999) and the limit of quantification was less than 10 ng · mL -1 The recoveries of three macrolide antibacterials and their metabolites ranged from 81.45% to 96.82% at 3 addition levels. The intra-day precision was less than 5.00% and the intra-day precision was less than 10.00%. Conclusion Qu ECHERS-LC-MS triple quadrupole mass spectrometry is simple, rapid, sensitive and specific for the determination of three macrolide antibiotics in plasma and its metabolites. It is suitable for the determination of macrolide Antibacterial drugs and their metabolites.