目的 建立測定含麥冬注射液中麥冬皂苷D（OPD）和麥冬皂苷D'（OPD'）含量的UPLC-MS/MS方法，評價不同廠家不同批次該注射液的質(zhì)量的均勻性，為該藥臨床的安全性評估提供實驗依據(jù)。方法 色譜采用ACQUITY UPLC HSS T3C₁₈色譜柱（100 mm×2.1 mm，1.7 μm）；流動相為0.1%甲酸水（A）-乙腈（B），梯度洗脫；體積流量為0.3 mL/min；進樣量為2 μL；質(zhì)譜采用電噴霧離子源（ESI），負離子檢測模式（-），通過多反應(yīng)監(jiān)測（MRM）同時對注射液中OPD和OPD'進行定量分析。結(jié)果 該注射液中OPD和OPD'在50~10 000 ng/mL線性關(guān)系均良好，r均大于0.995 7；專屬性，精密度，重復(fù)性和穩(wěn)定性良好。結(jié)論 不同廠家注射液樣本之間存在一定的質(zhì)量差異，同一樣本中OPD和OPD'以一定比例共存；OPD和OPD'混合給藥對紅細胞的溶血作用遠高于OPD'單獨給藥，OPD'最高理論平均血藥濃度雖未達溶血率濃度警戒線，但臨床使用仍可能具有一定風險并對機體產(chǎn)生不良反應(yīng)，應(yīng)給予高度重視。

Objective To establish a simultaneous quantitative analytical method of ophiopogonin D (OPD) and ophiopogonin D' (OPD') in the tested sample contains Ophiopogon japonicas based on ultra-high performance liquid chromatography coupled with electrospray tandem mass spectrometry (UPLC-MS/MS), assessed of the quality homogeneity of different factory and different batches injections, to provide the data reference for its clinical safety assessment from a hemolytic perspective around the OPD' toxic effects. Method The chromatographic separation was performed on an ACQUITY UPLC HSS T3 C₁₈ column (100 mm×2.1 mm,1.7 μm) with a gradient elution of 0.1% formic acid in water and acetonitrile at a flow rate of 0.3 mL/min, and the injection volume was 2 μL. The two components were detected using an electrospray ionization source in negative ionization mode (ESI-) and quantified by multiple reaction monitor (MRM) scanning at the same time. Result The OPD and OPD' both had good linear relationship in range of 50-10 000 ng/mL, the value of "r" was all more than 0.995 7, the specificity, linearity, precision, repeatability, stability and durability of the method were all good. Conclusion The qualities of different factory of the injection have differences in various degrees, OPD and OPD' co-exist in a certain proportion in the same sample, though the theory highest average blood drug concentration not a cordon of hemolysis rate, clinical application still likely to have a certain risk and adverse effects on the body which should be given high attention.

R282.71;R965.3

國家科技重大專項（2015ZX09501004）