基于二维液相色谱法测定关节假体周围感染患者关节液中万古霉素的质量浓度  

Measurement of vancomycin concentration in synovial fluid in patients with periprosthetic joint infection by two-dimensional liquid chromatography

作　　者：黄俊杰 常军民[1] 何家伟[2,3,5] 汪洋 纪保超[4] 赵军[2,3,5] HUANG Junjie;CHANG Junmin;HE Jiawei;WANG Yang;JI Baochao;ZHAO Jun(College of Pharmacy,Xinjiang Medical University,Urumqi 830017,China;Department of Pharmacy,the First Affiliated Hospital of Xinjiang Medical University,Urumqi 830054,China;Xinjiang Key Laboratory of Clinical Drug Research,Urumqi 830054,China;Department of Orthopaedics,the First Affiliated Hospital of Xinjiang Medical University,Urumqi 830054,China;Engineering Research Center of Xinjiang and Central Asian Medicine Resources,Ministry of Education,Urumqi 830017,China)

机构地区：[1]新疆医科大学药学院,乌鲁木齐830017 [2]新疆医科大学第一附属医院药学部,乌鲁木齐830054 [3]新疆药物临床研究重点实验室,乌鲁木齐830054 [4]新疆医科大学第一附属医院关节外科,乌鲁木齐830054 [5]新疆及中亚特色医药资源教育部工程研究中心,乌鲁木齐830017

出　　处：《西北药学杂志》2025年第1期107-113,共7页Northwest Pharmaceutical Journal

基　　金：新疆维吾尔自治区自然科学基金项目(编号:2022D01C240);武汉药学会第二届医院药学学科发展项目(编号:WHPA202305011);新疆维吾尔自治区“天山英才”医药卫生高层次人才培养计划项目(编号:TSYC202301A051)。

摘　　要：目的基于二维液相色谱法(two-dimensional liquid chromatography,2D-LC)建立检测关节假体周围感染(prosthetic joint infection,PJI)患者关节液中万古霉素质量浓度的方法。方法采用FLC2701型2D-LC系统对万古霉素进行2D分离,第一维液相色谱系统采用Aston SC2-1A色谱柱(3.5 mm×25 mm,5μm),流动相为甲醇-乙腈-10 mmoL·L^(−1)磷酸铵水溶液(1∶1∶10),流速为0.6 mL·min^(−1);第二维液相色谱系统采用Aston SCB色谱柱(4.6 mm×125 mm,5μm),流动相为1.0 mmoL·L^(−1)磷酸氢二铵水溶液(pH=7.4)-1.0 mmoL·L^(−1)磷酸氢二铵水溶液(pH=3.0)-乙腈(52∶37∶11),流速为1.2 mL·min^(-1);柱温为45℃;检测波长为232、279 nm;进样量为50μL。结果关节假体周围感染患者关节液中万古霉素的质量浓度在1.01~50.28μg·mL^(−1)范围内线性关系良好(r=0.9998),该方法日内、日间精密度RSD值均<2.26%,平均回收率为93.83%~100.16%,样品提取回收率为100.76%~103.01%,样品稳定性RSD值<2.28%。结论基于2D-LC建立的关节假体周围感染患者关节液中万古霉素质量浓度测定方法简便、准确、高效,可用于临床患者关节液中万古霉素的质量浓度监测。Objective A method based on two-dimensional liquid chromatography(2D-LC)was established for the concentration of vancomycin in the synovial fluid of patients with periprosthetic joint infection(PJI).Methods The 2D separation of vancomycin was carried out using a FLC27012D-LC system,and the first-dimensional liquid chromatography system was an Aston SC2-1A column(3.5 mm×25 mm,5μm),with a mobile phase of methanol-acetonitrile-10 mmoL·L^(−1) aqueous ammonium phosphate solution(1∶1∶10)at a flow rate of 0.6 mL·min^(−1);the second-dimensional liquid chromatography system was an Aston SCB(4.6 mm×125 mm,5μm),and the mobile phase was 1.0 mmoL·L^(−1) diammonium phosphate(pH=7.4)-1.0 mmoL·L^(−1) diammonium phosphate(pH=3.0)-acetonitrile(52∶37∶11)at a flow rate of 1.2 mL·min^(−1);the column temperature was 45℃;the detection wavelengths were 232 and 279 nm;and the injection volume was 50μL.Results The mass concentration of vancomycin in the synovial fluid of the patients was linear in the range of 1.01—50.28μg·mL^(−1)(r=0.9998),and the RSD values of intra-day and inter-day precision of this method were both<2.26%,the average recoveries were in the range of 93.83%—100.16%,the recoveries of sample extraction were in the range of 100.76%—103.01%,and the sample stability RSD values were all<2.28%.Conclusion The method for the determination of vancomycin concentration in the joint fluid of patients with periprosthetic infection based on 2D-LC is simple,accurate and efficient,and can be used to monitor the concentration of vancomycin in the joint fluid of clinical patients.

关 键 词：二维液相色谱法 关节假体周围感染 关节液 万古霉素 

分 类 号：R917[医药卫生—药物分析学]