Journal of Chromatography B ( IF 2.8 ) Pub Date : 2021-01-18 , DOI: 10.1016/j.jchromb.2021.122522 Xiufang Liang , Zhongping Gou , Xiandi Wang , Yongsheng Wang , Jiao Yue , Na Li , Ping Feng , Yongping Qin , Jiancheng Zeng
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 D3-cefuroxime and D3,13C-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.
中文翻译:
通过UPLC-MS / MS同时定量测定人腰椎纤维环,髓核和血清中的头孢呋辛和克林霉素
背景
这项研究旨在开发一种灵敏,准确的方法,用于同时定量测定人血清,腰椎纤维环和髓核中的头孢呋辛和克林霉素。
方法
在三重四极杆AB Qtrap 5500系统上,在正离子模式下,通过多反应监测模式下的超高效液相色谱-电喷雾串联质谱法对头孢呋辛和克林霉素进行定量。内部标准分别为d 3 -cefuroxime和d 3,13 C-克林霉素。通过沉淀总蛋白对样品进行预处理。
结果
该方法在头孢呋辛的100至100,000 ng / mL和克林霉素的10至10,000 ng / mL的宽校正范围,头孢呋辛和1对1的10,000至10000 ng / mL的宽校正范围内显示出高灵敏度和良好的线性腰椎髓核中克林霉素的浓度为000 ng / mL。在所有样品类型中,两种分析物的相关系数均大于0.99,日内和日间精度(相对标准偏差)小于15%,精度(相对误差)在14%以内。该方法有效地定量了斜腰椎间融合手术患者中头孢呋辛和克林霉素的渗透率。
结论
已开发出一种用于同时检测头孢呋辛和克林霉素的非常灵敏,特异的方法,用于检测人类腰椎纤维环,髓核和血清样品。