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Simultaneous determination of multiclass antibiotics in sewage sludge based on QuEChERS extraction and liquid chromatography-tandem mass spectrometry
Analytical Methods ( IF 2.7 ) Pub Date : 2019/12/27 , DOI: 10.1039/c9ay02188d Akinranti S. Ajibola 1, 2, 3, 4, 5 , Selina Tisler 1, 2, 3, 4, 5 , Christian Zwiener 1, 2, 3, 4, 5
Analytical Methods ( IF 2.7 ) Pub Date : 2019/12/27 , DOI: 10.1039/c9ay02188d Akinranti S. Ajibola 1, 2, 3, 4, 5 , Selina Tisler 1, 2, 3, 4, 5 , Christian Zwiener 1, 2, 3, 4, 5
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A modified quick, easy, cheap, effective, rugged and safe (QuEChERS) based methodology with a dispersive solid-phase extraction (d-SPE) clean-up followed by liquid chromatography-triple quadrupole mass spectrometry analysis was developed and validated for simultaneous determination of seventeen multiclass antibiotics in sewage sludge. The target antibiotics included four sulfonamides, three fluoroquinolones, three macrolides, two tetracyclines, three β-lactams, trimethoprim and thiamphenicol. Extraction solvents, buffer salts and d-SPE sorbents were optimized. Chromatographic separation of target antibiotics was performed on a Poroshell EC-C18 column while detection and quantification were achieved with a triple quadrupole mass spectrometer using electrospray ionization in both positive and negative modes by fast polarity switching. The method limits of detection ranged from 0.003 ng g−1 dw (trimethoprim) to 120 ng g−1 dw (oxytetracycline). Intra-day precision of less than 18% (% RSD) was achieved. The applied d-SPE clean-up was effective for reducing matrix effects due to co-extracted components. The method was successfully applied for measurements of target antibiotics in sewage sludge samples from three wastewater treatment plants (WWTPs) in Nigeria. Except for β-lactam antibiotics which were not recovered during the method development, most target antibiotics were detected in the sludge samples. The highest concentrations were found for tetracyclines (up to 4689 ng g−1 dw for oxytetracycline) and fluoroquinolones (up to 1201 ng g−1 dw for ciprofloxacin). This work expands our knowledge on the applicability of QuEChERS method for the extraction of antibiotic residues from sewage sludge. The findings revealed the ubiquitous presence of the majority of the target antibiotics in the investigated Nigerian WWTPs.
中文翻译：
QuEChERS萃取-液相色谱-串联质谱法同时测定污水污泥中的多种抗生素
开发了一种改进的快速，简便，廉价，有效，坚固和安全的（QuEChERS）方法，并进行了分散固相萃取（d-SPE）净化，然后进行液相色谱-三重四极杆质谱分析，并进行了同时测定的验证污泥中的十七种多类抗生素中的一种。目标抗生素包括四种磺酰胺类，三种氟喹诺酮类，三种大环内酯类，两种四环素类，三种β-内酰胺类，甲氧苄啶和甲砜霉素。优化了萃取溶剂，缓冲盐和d-SPE吸附剂。在Poroshell EC-C18色谱柱上进行目标抗生素的色谱分离，同时使用三极四极杆质谱仪通过快速极性切换，在正负两种模式下使用电喷雾电离进行检测和定量。-1 dw（甲氧苄啶）至120 ng g -1 dw（土霉素）。日内精度低于18％（RSD％）。施加的d-SPE净化可有效减少因共萃取组分而产生的基质效应。该方法已成功应用于尼日利亚三个污水处理厂（WWTP）污水污泥样品中目标抗生素的测量。除了在方法开发过程中未回收的β-内酰胺抗生素外，污泥样品中还检测到了大多数目标抗生素。四环素（土霉素为4689 ng g -1 dw）和氟喹诺酮类药物（最高为1201 ng g -1）的最高浓度环丙沙星的dw）。这项工作扩展了我们对QuEChERS方法从污水污泥中提取抗生素残留物的适用性的认识。研究结果表明，在调查的尼日利亚污水处理厂中，大多数目标抗生素普遍存在。
更新日期：2020-02-13
中文翻译：
QuEChERS萃取-液相色谱-串联质谱法同时测定污水污泥中的多种抗生素
开发了一种改进的快速，简便，廉价，有效，坚固和安全的（QuEChERS）方法，并进行了分散固相萃取（d-SPE）净化，然后进行液相色谱-三重四极杆质谱分析，并进行了同时测定的验证污泥中的十七种多类抗生素中的一种。目标抗生素包括四种磺酰胺类，三种氟喹诺酮类，三种大环内酯类，两种四环素类，三种β-内酰胺类，甲氧苄啶和甲砜霉素。优化了萃取溶剂，缓冲盐和d-SPE吸附剂。在Poroshell EC-C18色谱柱上进行目标抗生素的色谱分离，同时使用三极四极杆质谱仪通过快速极性切换，在正负两种模式下使用电喷雾电离进行检测和定量。-1 dw（甲氧苄啶）至120 ng g -1 dw（土霉素）。日内精度低于18％（RSD％）。施加的d-SPE净化可有效减少因共萃取组分而产生的基质效应。该方法已成功应用于尼日利亚三个污水处理厂（WWTP）污水污泥样品中目标抗生素的测量。除了在方法开发过程中未回收的β-内酰胺抗生素外，污泥样品中还检测到了大多数目标抗生素。四环素（土霉素为4689 ng g -1 dw）和氟喹诺酮类药物（最高为1201 ng g -1）的最高浓度环丙沙星的dw）。这项工作扩展了我们对QuEChERS方法从污水污泥中提取抗生素残留物的适用性的认识。研究结果表明，在调查的尼日利亚污水处理厂中，大多数目标抗生素普遍存在。
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