色谱

色谱 ›› 2018, Vol. 36 ›› Issue (11): 1112-1118.DOI: 10.3724/SP.J.1123.2018.07007

• 研究论文 • 上一篇    下一篇

TiO2修饰磁性石墨烯-通过型固相萃取净化人血中氯霉素、甲砜霉素和氟甲砜霉素

何世伟1, 赵永纲1,2, 朱岩1   

  1. 1. 浙江大学化学系, 浙江 杭州 310027;
    2. 宁波市疾病预防控制中心, 浙江 宁波 315010
  • 收稿日期:2018-07-05 出版日期:2018-11-08 发布日期:2014-09-30
  • 通讯作者: 朱岩.E-mail:zhuyan@zju.edu.cn.
  • 基金资助:

    浙江省基础公益研究计划项目（LGF18B050003）.

Nano-titania-coated modified magnetic graphene oxide for pass-through cleanup of chloramphenicol, thiamphenicol, and florfenicol in human blood

HE Shiwei1, ZHAO Yonggang1,2, ZHU Yan1   

  1. 1. Department of Chemistry, Zhejiang University, Hangzhou 310027, China;
    2. Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China
  • Received:2018-07-05 Online:2018-11-08 Published:2014-09-30
  • Supported by:

    Zhejiang Provincial Program for Public Welfare of Technology Application Research Plan (No. LGF18B050003).

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摘要：

采用TiO2修饰磁性石墨烯作为通过型固相萃取柱填料，并用于净化去除血液样品中磷脂类物质的干扰，建立了一种快速、高效、准确的测定人血中残留氯霉素、甲砜霉素与氟甲砜霉素的超快速液相色谱-串联质谱分析方法。样品经乙腈提取，使用TiO2修饰磁性石墨烯-通过型固相萃取柱进行净化处理，以Eclipse Plus C18色谱柱（100 mm×2.1 mm，1.8 μm）分离，以0.08%（v/v）氨水溶液与0.08%（v/v）氨水乙腈溶液为流动相梯度洗脱，电喷雾离子源多反应监测负离子模式下检测，采用内标法定量。3种目标化合物在0.1~10.0 μg/L范围内具有良好的线性（决定系数r2>0.999），定量限（S/N>10）为0.056~0.082 μg/L，目标化合物的加标回收率为90.0%~105%，相对标准偏差为1.2%~6.6%。该方法可用于临床血样中残留氯霉素、甲砜霉素与氟甲砜霉素的快速筛查和确证分析。

关键词: TiO2修饰磁性石墨烯, 氟甲砜霉素, 甲砜霉素, 氯霉素, 人血, 通过型固相萃取柱, 液相色谱-串联质谱

Abstract:

To develop a rapid, effective, and accurate method for the simultaneous determination of chloramphenicol, thiamphenicol, and florfenicol in human blood by pass-through cleanup solid-phase extraction combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS), novel nano-titania-coated modified magnetic graphene oxide (TiO2-Mag-GO) is used as the PRiME pass-through cleanup solid-phase extraction sorbent for the cleanup of blood phospholipids. The chromatographic separation was performed on an Eclipse Plus C18 column (100 mm×2.1 mm, 1.8 μm) using 0.08% (v/v) aqueous ammonia solution and acetonitrile having aqueous ammonia (0.08%, v/v) as mobile phases. The tandem mass spectrometer was operated using electrospray ion source (ESI) in the multiple reaction monitoring (MRM) mode. The results showed that the linearities were in the range of 0.1-10.0 μg/L with the determination coefficients (r2) greater than 0.9990 for chloramphenicol, thiamphenicol, and florfenicol. The limits of quantification (LOQs) (S/N>10) in the blood samples were between 0.056 and 0.082 μg/L and the recoveries ranged from 90.0% to 105% at three spiked levels. Precision values expressed as relative standard deviations (RSDs) were in the range of 1.2%-6.6%. The developed method can be used for routine analyses to determine chloramphenicol, thiamphenicol, and florfenicol in clinical studies.

Key words: chloramphenicol, florfenicol, human blood, liquid chromatography-tandem mass spectrometry (LC-MS/MS), nano-titania-coated modified magnetic graphene oxide (TiO2-Mag-GO), pass-through cleanup, thiamphenicol

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