| 二维液相色谱法测定脑脊液中替加环素浓度及其临床应用 |
| 投稿时间：2020-03-08 修订日期：2020-05-14 点此下载全文 |
| 引用本文：程彩奕,邓冬梅,王显凤,杨征,幸海燕.二维液相色谱法测定脑脊液中替加环素浓度及其临床应用[J].药学实践杂志,2020,38(6):543~546 |
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| 基金项目:重庆市社会科学规划培育项目（2018PY79）；陆军军医大学临床科研项目（2018XLC3072）；陆军特色医学中心人才创新能力培养计划（2019CXLCC013） |
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| 中文摘要:目的 建立二维液相色谱法检测人脑脊液中替加环素浓度，用于颅内感染患者的药物浓度监测。方法 采用外标法定量，第一维色谱柱为Aston SNX5苯基色谱柱（50 mm×4.6 mm，5 μm），流动相为磷酸铵（氨水调pH7.5）-甲醇（45:55，V/V），流速1.0 ml/min。第二维色谱柱为Aston SC5 C18色谱柱（275 mm×4.6 mm，5 μm），流动相为磷酸铵（氨水调pH7.4）-磷酸铵（氨水调pH3.0）-乙腈（30:50:20，V/V/V），流速1.2 ml/min。检测波长340 nm，色谱柱温40 ℃，进样量：200 μl。结果 脑脊液中替加环素64.5～1 290.0 ng/ml内与峰面积呈良好线性关系（r=0.999 8）；日内、日间精密度RSD<5%，准确度为98.80%～106.51%。结论 该方法操作简便、快速、准确、灵敏，适用于临床人脑脊液替加环素的浓度监测，可为颅内感染患者的个体化给药提供科学依据。 |
| 中文关键词:替加环素 二维液相色谱法 颅内感染 药物监测 脑脊液 |
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| Determination of tigecycline in human cerebrospinal fluid by two-dimensional liquid chromatography and its clinical application |
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| Abstract:Objective To establish a two-dimensional high-performance liquid chromatography method for the determination of tigecycline in human cerebrospinal fluid, which can be used for the drug monitoring in patients with intracranial infection.Methods The quantification was carried out by an external standard method. The first-dimension column was a Aston SNX5 phenyl chromatographic column (50 mm×4.6 mm, 5 μm) with ammonium phosphate (pH was adjusted with ammonium hydroxide to 7.5)-methanol (45∶55, V/V) as the mobile phase and the flow rate was 1.2 ml/min. The second-dimension chromatographic column was Aston SC5 C18 (275 mm×4.6 mm, 5 μm), with ammonium phosphate (pH was adjusted with ammonium hydroxide to 7.4)-ammonium phosphate (pH was adjusted with ammonium hydroxide to 3.0)- acetonitrile (30∶50∶20, V/V/V) as the mobile phase and the flow rate was 1.0 ml/min. The detection wavelength was 340 nm. The temperature was 40 ℃ and the injection volume was 200 μl.Results The calibration curve of tigecycline showed good linearity from 64.5 to 1 290.0 ng/ml in human cerebrospinal fluid (r=0.999 8). The RSD of intra and inter-day precision were less than 5.0% with the detection accuracy of 98.80%−106.51%.Conclusion This method is simple, quick, accurate, specific and sensitive. It meets the requirements of tigecycline determination in clinical human cerebrospinal fluid, which offers the individualized therapeutic assurance for patients with intracranial infection. |
| keywords:tigecycline two-dimensional high-performance liquid chromatography intracranial infection drug monitoring cerebrospinal fluid |
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