张佳成,詹达强,毕重文,袁恒杰
AuthorsHTML:张佳成，詹达强，毕重文，袁恒杰
AuthorsListE:Zhang Jiacheng,Zhan Daqiang,Bi Chongwen,Yuan Hengjie
AuthorsHTMLE:Zhang Jiacheng，Zhan Daqiang，Bi Chongwen，Yuan Hengjie
Unit:天津医科大学总医院，天津 300052
Unit_EngLish:General Hospital of Tianjin Medical University，Tianjin 300052，China
Abstract_Chinese:采用超高效液相-串联质谱联用建立人血浆中地塞米松含量的检测方法．色谱柱为 BEH C18，流动相为 0.01%甲酸乙腈溶液-0.01%甲酸水溶液，梯度洗脱，流速为 0.4 mL/min，电喷雾正离子模式，多反应监测．调谐后， 地塞米松定量分析检测的离子对为 m/z 393.03 → 237.02．地塞米松在 1.28～312.12 ng/mL(r2＝0.998 8)质量浓度范 围内与色谱峰面积线性关系良好；检测限和定量下限分别为 0.50 ng/mL 和 1.00 ng/mL；日内精密度和日间精密度 RSD 均小于 10.01%，准确度为 100.65%～107.82%；提取回收率为 80.90%～84.32%；基质效应为 102.4%～120.0%； 在多种试验条件下，血浆样品稳定性良好，相对误差均在±10%之内．由患有干燥综合征的妊娠母亲抗 SSA/Ro 或 抗 SSB/La 抗体阳性所引起的免疫性胎儿房室传导阻滞目前临床上采用皮质类固醇治疗，但缺乏与药物疗效及安全 性等内容有关的具体数据．本方法首次成功用于患有干燥综合征的妊娠母亲口服地塞米松治疗免疫性胎儿完全性房 室传导阻滞病例，在新生儿体内定性和定量检测到 DXM 原形药物，分娩后同时定量检测母亲及新生儿血浆样品中 地塞米松质量浓度分别为 25.7 ng/mL 和 5.6 ng/mL，比例约为 5∶1．本方法灵敏度高、准确性好、方便快捷，可同 时测定母亲和新生儿血浆中地塞米松的浓度，为临床治疗提供精准的数据支撑，同时为进行系统全面的数据分析打 下基础，确保患者用药安全有效．
Abstract_English:We aimed to develop an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLCMS/MS)method to determine the concentration of dexamethasone (DXM)in human plasma. The column was an ethylene bridged hybrid C18 eluted with a gradient of 0.01% formic acid in acetonitrile-0.01% formic acid in water as the mobile phase at a flow rate of 0.4 mL/min in electrospray ionization positive ion mode with multiple reaction monitoring. After tuning，the ion pair for quantification was DXM：m/z 393.03→237.02. DXM showed a good linear relationship within the range of 1.28～312.12 ng/mL(r2＝0.998 8). The detection limit and lower limit of quantification were 0.50 ng/mL and 1.00 ng/mL，respectively. Relative standard deviations of intra-day and inter-day precision were ＜10.01%. Accuracy was within the range of 100.65%—107.82%. Extraction recovery was within the range of 80.90%—84.32%. The matrix effects ranged from 102.4% to 120.0%. Plasma samples remained stable before and after treatment under various conditions，with the relative error being within ±10%. Fetal immune mediated atrioventricular block induced by anti-SSA/Ro-positive or anti-SSB/La-positive mothers with Sjogren syndrome wereclinicallytreated with corticosteroids，whereas the effect and security need to be testified. This is the first applied method in cases in which the mother is administered DXM orally. It was found that DXM exists in neonate plasma and that the DXM concentrations of plasma samples of the mother and neonate were 25.7 ng/mL and 5.6 ng/mL，respectively， with rough ratio being 5∶1. The developed method is sensitive，efficient，and convenient to determine the concentration of DXM in plasma of mother and neonate so as to provide precise data for clinical application.
Keyword_Chinese:地塞米松；房室传导阻滞；超高效液相-串联质谱联用
Keywords_English:dexamethasone；atrioventricular block；ultra-high performance liquid chromatography-tandem mass spectrometry

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