Yao Fen, Wang Yifan, Hou Yating, Wang Xipei, Lan Jinhua, Wu Zheng, Wang Yirong, Chen Chunbo
School of Biology and Biological Engineering, South China University of Technology, Guangzhou 510006, Guangdong, China.
Department of Emergency Medicine, Maoming People's Hospital, 101 Weimin Road, Maoming 525000, Guangdong, China.
Int J Anal Chem. 2020 Dec 29;2020:6671392. doi: 10.1155/2020/6671392. eCollection 2020.
Utilizing tigecycline-d9 as an internal standard (IS), we establish and validate a simple, effective, and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantitative measurement of tigecycline (TGC) in patient plasma. Acetonitrile was used as a precipitant to process plasma samples by a protein precipitation method. The analyte and IS were separated on an HSS T3 (2.1 × 100 mm, 3.5 m) chromatographic column using isocratic program with a mobile phase comprising of 80% solvent A (water containing 0.1% formic acid (v/v) with 5 mM ammonium acetate) and 20% solvent B (acetonitrile) with a flow rate of 0.3 mL/min. The mass spectrometer, scanning in multireaction monitoring (MRM) mode and using an electrospray ion source (ESI), operated in the positive-ion mode. The ion pairs used for quantitative analysis were / 586.4 ⟶ 513.3 and / 595.5 ⟶ 514.3 for TGC and the IS, respectively. The range of the linear calibration curve obtained with this approach was 50-5000 ng/ml. Intra- and interbatch precision for TGC quantitation were less than 7.2%, and the accuracy ranged from 93.4 to 101.8%. The IS-normalized matrix effect was 87 to 104%. Due to its high precision and accuracy, this novel method allows for fast quantitation of TGC with a total analysis time of 2 min. This approach was effectively applied to study the pharmacokinetics of TGC in critically ill adult patients.
以替加环素 - d9作为内标（IS），我们建立并验证了一种简单、有效且快速的液相色谱 - 串联质谱（LC - MS/MS）方法，用于定量测定患者血浆中的替加环素（TGC）。使用乙腈作为沉淀剂，通过蛋白质沉淀法处理血浆样本。分析物和内标在HSS T3（2.1×100 mm，3.5μm）色谱柱上分离，采用等度洗脱程序，流动相由80%的溶剂A（含0.1%甲酸（v/v）和5 mM醋酸铵的水）和20%的溶剂B（乙腈）组成，流速为0.3 mL/min。质谱仪在多反应监测（MRM）模式下扫描，使用电喷雾离子源（ESI），以正离子模式运行。用于定量分析的离子对分别为TGC的 / 586.4⟶ 513.3和内标的 / 595.5⟶ 514.3。用该方法获得的线性校准曲线范围为50 - 5000 ng/ml。TGC定量的批内和批间精密度均小于7.2%，准确度范围为93.4%至101.8%。内标归一化基质效应为87%至104%。由于其高精度和准确性，这种新方法能够快速定量TGC，总分析时间为2分钟。该方法有效地应用于研究危重症成年患者中TGC的药代动力学。
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