| 离心超滤结合超高效液相色谱串联质谱法测定人血浆中替考拉宁游离浓度 |
| 投稿时间：2020-03-28 修订日期：2020-08-06 点此下载全文 |
| 引用本文：付文倩,张敏新,姚囡囡,张丽丽,宋洪涛.离心超滤结合超高效液相色谱串联质谱法测定人血浆中替考拉宁游离浓度[J].药学实践杂志,2020,38(6):547~551 |
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| 基金项目:联勤保障部队第九〇〇医院院内课题基金项目（2018J19） |
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| 中文摘要:目的 建立离心超滤结合超高效液相色谱串联质谱法用以测定替考拉宁血浆游离浓度。方法 利用Centrifree®超过滤装置去除血浆中的白蛋白，超滤液直接进样测定替考拉宁游离浓度。色谱柱为EndeadvorsilTM C18柱（50 mm×2.1 mm，1.8 μm），流动相为0.02 mol/L醋酸铵溶液（含0.1%甲酸）与乙腈，梯度洗脱，在电喷雾离子化（ESI）正离子模式下进行检测。结果 替考拉宁血浆游离浓度为0.10～8.00 μg/ml，线性范围良好（r=0.999）。批内、批间精密度不超过7.00%，方法回收率为97.9%，基质效应因子为0.97。结论 该研究建立的方法简便、快速、灵敏、准确，可为临床开展替考拉宁血浆游离浓度监测提供依据。 |
| 中文关键词:替考拉宁 游离浓度 离心超滤 超高效液相色谱串联质谱法 |
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| Assay of unbound teicoplanin in human plasma by centrifugal ultrafiltration combined with ultra performance liquid chromatography-tandem mass spectrometry |
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| Abstract:Objective To establish an assay method for unbound teicoplanin in plasma by centrifugal ultrafiltration combined with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).Methods Protein was removed from plasma by a Centrifree® ultrafiltration device. The ultrafiltrate was injected to determine the unbound concentration of teicoplanin. EndeadvorsilTM C18 column (1.8 μm, 50 mm×2.1 mm) was used with gradient elution of acetonitrile and 0.02 mol/L ammonium acetate solution (containing 0.1% formic acid). The detection was performed on a triple-quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM)mode via electro spray ionization (ESI).Results The calibration curve of unbound teicoplanin in plasma was linear over the range of 0.10 to 8.00 μg/ml (r=0.999). The intra-assay precision and the inter-assay precision of samples didn't exceed 7.00%. The average relative recovery ratio was 97.9%, and the matrix effect factor was 0.97. The samples had good stability after being stored at room temperature for 10 h or at -20 ℃ for 15 days, and freeze-thawed 3 times (RSDs were all within 6.50%).Conclusion This method is convenient, fast, sensitive and accurate. It provided a basis for clinical development of teicoplanin unbound concentration monitoring. |
| keywords:teicoplanin unbound concentration centrifugal ultrafiltration ultra performance liquid chromatography-tandem mass spectrometry |
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