Analysis of trimethoprim, lincomycin, sulfadoxin and tylosin in swine manure using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry.
Analysis of trimethoprim, lincomycin, sulfadoxin and tylosin in swine manure using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry.
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采用激光二极管热解吸-大气压化学电离-串联质谱法分析猪粪中的甲氧苄啶、林可霉素、磺胺多辛和泰乐菌素。
DOI：
10.1016/j.talanta.2014.04.023
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发表时间：
2014
期刊：
影响因子：
--
通讯作者：
S. Sauvé
中科院分区：
文献类型：
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作者：
Morgan Solliec;D. Massé;S. Sauvé
建立了一种新的提取-高通量样品分析技术，用于4种兽用抗生素的测定。分析物属于不同的抗生素组，例如化疗药物、磺胺类、林可酰胺类和大环内酯类。采用超声提取法从冻干粪便中提取甲氧苄氨嘧啶（TMP）、磺胺多辛（SFX）、林可霉素（LCM）和泰乐菌素（TYL）。采用McIlvaine缓冲液和甲醇（MeOH）作为提取缓冲液，然后用阳离子交换固相萃取（SPE）进行净化。采用激光二极管热解吸-大气压化学电离（LDTD-APCI）串联质谱（MS/MS）和选择反应监测（SRM）检测进行分析。LDTD是一种高通量进样方法，与使用传统液相色谱法（LC）时的几分钟相比，它将每个样品的总分析时间缩短至不到15秒。样品萃取后，优化了各种SPE参数：固定相，萃取溶剂的组成，提取的样品量和样品pH值。LDTD参数也进行了优化：溶剂沉积，载气，激光功率和电晕放电。方法检测限（MLD）范围为2.5 - 8.3 µg kg− 1，方法定量限（MLQ）范围为8.3 - 28 µg kg−1。粪便基质中的校准曲线显示所有分析物的良好线性（R2≥0.996），日间和日内变异系数低于14%。从粪便中回收的分析物范围从53%到69%。该方法已成功地应用于真实的粪便样品。
A new extraction method coupled to a high throughput sample analysis technique was developed for the determination of four veterinary antibiotics. The analytes belong to different groups of antibiotics such as chemotherapeutics, sulfonamides, lincosamides and macrolides. Trimethoprim (TMP), sulfadoxin (SFX), lincomycin (LCM) and tylosin (TYL) were extracted from lyophilized manure using a sonication extraction. McIlvaine buffer and methanol (MeOH) were used as extraction buffers, followed by cation-exchange solid phase extraction (SPE) for clean-up. Analysis was performed by laser diode thermal desorption-atmospheric pressure chemical-ionization (LDTD-APCI) tandem mass spectrometry (MS/MS) with selected reaction monitoring (SRM) detection. The LDTD is a high throughput sample introduction method that reduces total analysis time to less than 15 s per sample, compared to minutes when using traditional liquid chromatography (LC). Various SPE parameters were optimized after sample extraction: the stationary phase, the extraction solvent composition, the quantity of sample extracted and sample pH. LDTD parameters were also optimized: solvent deposition, carrier gas, laser power and corona discharge. The method limit of detection (MLD) ranged from 2.5 to 8.3 µg kg−1while the method limit of quantification (MLQ) ranged from 8.3 to 28 µg kg−1. Calibration curves in the manure matrix showed good linearity (R2≥0.996) for all analytes and the interday and intraday coefficients of variation were below 14%. Recoveries of analytes from manure ranged from 53% to 69%. The method was successfully applied to real manure samples.