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目的建立在线样品处理技术和液相色谱-串联质谱法测定人血浆中依普黄酮(雌激素抗骨质疏松药物)浓度的方法。方法血浆样品稀释后,直接用HPLC二维系统完成在线预处理和分离。使用前处理柱为Shim-Pack MAYI-ODS柱,流动相为纯水-甲醇梯度配比,分析柱为Dikma Diamonsil C18色谱柱,流动相为0.2%甲酸水溶液-甲醇=15∶85,通过电喷雾离子化三重四级杆质谱,经多反应检测正离子模式进行检测。结果依普黄酮的血药浓度在0.5～250.0 ng.mL-1线性良好(γ=0.999),检测限在0.5 ng.mL-1,提取回收率在81%～88%,日内、日间精密度均在(RSD)≤11.6%,准确度在87.6%～113.7%。结论该法操作快速高效、灵敏准确、重现性好,能够满足临床药代动力学研究的需要。
OBJECTIVE: To establish a method for on-line sample processing and liquid chromatography-tandem mass spectrometry for the determination of Ipraflatone (estrogen-anti-osteoporosis drug) in human plasma. Methods After the plasma samples were diluted, the two-dimensional system of HPLC was used to complete online pretreatment and separation. The column was Shim-Pack MAYI-ODS. The mobile phase consisted of pure water-methanol gradient. The analytical column was Dikma Diamonsil C18 and the mobile phase consisted of 0.2% formic acid in water-methanol = 15:85. Ionization triple quadrupole mass spectrometry, multi-reaction detection positive mode detection. Results The plasma concentration of ipriflavone was good at 0.5-250.0 ng · mL-1 (γ = 0.999). The detection limit was 0.5 ng.mL-1 and the recovery was 81% -88%. The intra- and inter-day precision The degrees are (RSD) ≤ 11.6% with accuracy of 87.6% ~ 113.7%. Conclusion The method is fast and efficient, sensitive and accurate, reproducible, and can meet the needs of clinical pharmacokinetics.