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经 UPLC-MS/MS 法同时定量检测人腰椎纤维环、髓核和血清中的头孢呋辛和克林霉素。

Simultaneous quantification of cefuroxime and clindamycin in human lumbar anulus fibrosus, nucleus pulposus and serum via UPLC-MS/MS.

机构信息

Institute of Clinical Trials, West China Hospital, Sichuan University, Chengdu, Sichuan 610041, PR China.

Department of Orthopaedic Surgery and Orthopaedic Research Institute, West China Hospital, Sichuan University, Chengdu, Sichuan 610041, PR China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2021 Feb 15;1165:122522. doi: 10.1016/j.jchromb.2021.122522. Epub 2021 Jan 18.

DOI:10.1016/j.jchromb.2021.122522
PMID:33545501
Abstract

BACKGROUND

This study aimed to develop a sensitive, accurate method for simultaneously quantifying cefuroxime and clindamycin in human serum, lumbar anulus fibrosus and nucleus pulposus.

METHODS

Cefuroxime and clindamycin were quantified using ultra high-performance liquid chromatography-electrospray ionization tandem mass spectrometry in multiple-reaction-monitoring mode on a triple-quadrupole AB Qtrap 5500 system in positive ion mode. Internal standards were D-cefuroxime and DC-clindamycin. Samples were pretreated by precipitating total protein.

RESULTS

The method showed high sensitivity and good linearity over broad calibration ranges from 100 to 100 000 ng/mL for cefuroxime and 10 to 10 000 ng/mL for clindamycin in serum, and from 10 to 10 000 ng/mL for cefuroxime and 1 to 1 000 ng/mL for clindamycin in lumbar nucleus pulposus. In all sample types, correlation coefficients were greater than 0.99, intra- and inter-day precision (relative standard deviation) was less than 15%, and accuracy (relative error) was within 14% for both analytes. This method was effective at quantifying penetration of cefuroxime and clindamycin in patients undergoing oblique lumbar interbody fusion surgery.

CONCLUSIONS

A very sensitive, specific method for simultaneous detection of cefuroxime and clindamycin has been developed for human lumbar anulus fibrosus, nucleus pulposus and serum samples.

摘要

背景

本研究旨在开发一种灵敏、准确的方法,用于同时定量检测人血清、腰椎纤维环和髓核中的头孢呋辛和克林霉素。

方法

采用超高效液相色谱-电喷雾串联质谱三重四极杆 AB Qtrap 5500 系统,正离子模式下,多反应监测模式,以 D-头孢呋辛和 DC-克林霉素为内标,对样品进行预处理,沉淀总蛋白后,定量检测。

结果

该方法在 100-100 000ng/mL 范围内对血清中头孢呋辛和 10-10 000ng/mL 范围内对克林霉素,以及在 10-10 000ng/mL 范围内对腰椎髓核中头孢呋辛和 1-1 000ng/mL 范围内对克林霉素均具有较高的灵敏度和良好的线性关系。在所有样本类型中,相关系数均大于 0.99,日内和日间精密度(相对标准偏差)均小于 15%,头孢呋辛和克林霉素的准确度(相对误差)均在 14%以内。该方法可有效定量检测接受斜外侧腰椎椎间融合术患者中头孢呋辛和克林霉素的渗透情况。

结论

本研究建立了一种用于检测人腰椎纤维环、髓核和血清样本中头孢呋辛和克林霉素的灵敏、特异的检测方法。

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