在线固相萃取-高效液相色谱串联质谱法快速测定水中痕量氯霉素类抗生素  

Rapid determination of trace chloramphenicol antibiotics in water by online solid phase extraction coupled with high performance liquid chromatography tandem mass spectrometry

作　　者：彭君 满倩茹 黄钢 孔婷 周瑾瑾 叶鹏 何功秀[3] PENG Jun;MAN Qianru;HUANG Gang;KONG Ting;ZHOU Jinjin;YE Peng;HE Gongxiu(Geological Experiment and Testing Center of Hunan Province,Changsha 410007,China;Shimadzu Guangzhou Branch Company,Guangzhou 510656,China;Central South University of Forestry&Technology,Changsha 410004,China)

机构地区：[1]湖南省地质实验测试中心,长沙410007 [2]岛津广州分公司,广州510656 [3]中南林业科技大学,长沙410004

出　　处：《化学分析计量》2024年第10期16-22,共7页Chemical Analysis And Meterage

基　　金：湖南省自然资源科技计划项目(20230146ST);湖南省地质院科研项目(HNGSTP202214)。

摘　　要：建立一种新型在线固相萃取-超高效液相色谱-串联质谱分析方法,自动进行样品富集、净化、分离及检测,实现环境水中氯霉素、甲砜霉素、氟甲砜霉素的定量分析。系统由专属的大体积进样器进样2 mL环境水样到亲水亲油的HLB柱上进行富集和浓缩后进行分析,且整个分析时间仅需17 min;使用同位素标记的内标法定量目标物质,用于校正在线固相萃取过程中不可避免的损失和基质效应,以确保方法准确性,测定结果同传统方法吻合度高。各组分在质量浓度0.50~50.0 ng/L范围内与对应的色谱峰面积线性相关性好,相关系数均大于0.9995,检出限为0.030~0.12 ng/L。3种浓度的样品溶液分别平行测定6次,测试结果的相对标准偏差为1.60%~9.04%,样品加标回收率为85.0%~123.0%。该方法准确可靠、操作简捷、灵敏度高、分析速度快,为研究抗生素在生态环境中的时空分布和迁移转化提供技术支撑。A new online solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry analytical method was established,which can automatically perform sample enrichment,clean-up,separation and detection,to quantitatively analyze chloramphenicol,thiamphenicol and florfenicol in environmental water.2 mL environmental water samples were injected into the hydrophilic and lipophilic HLB column by a dedicated large volume sampler for enrichment and concentration before analysis,which only took 17 minutes.The target material was used to correct the inevitable loss and matrix effect in the online solid phase extraction process to ensure the accuracy of the method.The results were consistent with the traditional method.Each component had a good linearity with the corresponding chromatographic peak area in the mass concentration range of 0.50 to 50.0 ng/L,with the correlation coefficient r greater than 0.9995.And the detection limits were 0.030-0.12 ng/L.The sample solutions at three concentration levels were measured in parallel for 6 times,whose RSD were in the range of 1.60%-9.04%,and the standard recoveries were in the range of 85.0%-123.0%.The method is simple,sensitive and fast,which provides a technical support for the study of the temporal and spatial distribution,migration and transformation of antibiotics in the ecological environment.

关 键 词：在线固相萃取 高效液相色谱-串联质谱法 抗生素 水质 

分 类 号：O657[理学—分析化学]