Liu Hsiang-Yu, Lin Shu-Ling, Fuh Ming-Ren
Department of Chemistry, Soochow University, 70 Linhsi Road, Shihlin, 11102 Taipei, Taiwan.
Department of Chemistry, Soochow University, 70 Linhsi Road, Shihlin, 11102 Taipei, Taiwan.
Talanta. 2016 Apr 1;150:233-9. doi: 10.1016/j.talanta.2015.12.045. Epub 2015 Dec 18.
A poly(lauryl methacrylate-co-methacrylic acid-co-ethylene glycol dimethacrylate) [LMA-MAA-EDMA] monolithic column was used to simultaneously determine amphenicol antibiotics (chloramphenicol/CAP, thiamphenicol/TAP, and florfenicol/FF) in milk and honey samples by capillary liquid chromatography tandem mass spectrometry (LC-MS/MS). QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was optimized for sample pretreatment. Good linearity (0.1-15 ng g(-1)) and extraction recoveries (95.8-100.2% and 95.6-99.3% for milk and honey samples, respectively; n=3) with minor matrix effect (≦ 5% ion suppression) were obtained. Limits of detection were estimated at 0.02-0.045 ng g(-1). Good intra-day/inter-day precision (0.2-9.1%/0.3-8.7%) and accuracy (90.5-110.0%/93.4-109.3%) were achieved. With more than 200 analyses of real samples, no noticeable carry-over and deterioration of separation efficiency were observed using the monolithic column. The applicability of the developed QuEChERS-capillary LC-MS/MS method was demonstrated by determining the occurrence of CAP, TAP, and FF in various milk and honey samples.
采用聚（甲基丙烯酸月桂酯-甲基丙烯酸-乙二醇二甲基丙烯酸酯）[LMA-MAA-EDMA]整体柱，通过毛细管液相色谱串联质谱（LC-MS/MS）同时测定牛奶和蜂蜜样品中的氯霉素类抗生素（氯霉素/CAP、甲砜霉素/TAP和氟苯尼考/FF）。对QuEChERS（快速、简便、廉价、有效、耐用和安全）方法进行了优化用于样品预处理。获得了良好的线性关系（0.1 - 15 ng g⁻¹）和提取回收率（牛奶和蜂蜜样品分别为95.8 - 100.2%和95.6 - 99.3%；n = 3），基质效应较小（离子抑制≦5%）。检测限估计为0.02 - 0.045 ng g⁻¹。实现了良好的日内/日间精密度（0.2 - 9.1%/0.3 - 8.7%）和准确度（90.5 - 110.0%/93.4 - 109.3%）。通过对200多个实际样品的分析，使用整体柱未观察到明显的残留和分离效率下降。通过测定各种牛奶和蜂蜜样品中CAP、TAP和FF的含量，证明了所开发的QuEChERS-毛细管LC-MS/MS方法的适用性。
