Wen Ching-Hsuan, 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. 2017 Mar 1;164:85-91. doi: 10.1016/j.talanta.2016.11.006. Epub 2016 Nov 7.
In this study, the salting-out solvent extraction and dispersive solid-phase extraction (dSPE) clean-up steps in QuEChERS (quick, easy, cheap, effective, rugged, and safe) method were optimized to reduce matrix effect and efficiently extract target sulfonamides from a variety of edible animal tissues. The extracted sulfonamides were then analyzed using liquid chromatography tandem mass spectrometry (LC-MS/MS). Good extraction recoveries (74.0-100.3% in five different sources of animal tissues; n=3) with acceptable matrix effect (<10%, except for liver samples) were obtained using the proposed method. For the first time, a commercial ND-lipids cartridge was used to remove hydrophobic matrix components from fat-rich animal tissues in the clean-up step of QuEChERS. In addition, good linearity (0.125-12.5ngg) was observed using matrix-matched calibration (in beef). Limits of detection (LODs) were estimated at 0.01-0.03ngg in beef, pork, and chicken samples. For beef tripe and pig liver samples, the LODs were in the range of 0.02-0.04ngg. Good intra-day/inter-day precision (1.0-10.5%/0.4-8.0%) and accuracy (95.2-107.2%/97.8-102.1%) were also achieved using the modified QuEChERS for sample pretreatment. The applicability of the modified QuEChERS-LC-MS/MS method was demonstrated by determining the occurrence of target sulfonamides in various edible animal tissues for potential food safety analysis.
在本研究中,对QuEChERS(快速、简便、廉价、有效、耐用且安全)方法中的盐析溶剂萃取和分散固相萃取(dSPE)净化步骤进行了优化,以减少基质效应,并从各种可食用动物组织中高效提取目标磺胺类药物。然后使用液相色谱串联质谱法(LC-MS/MS)对提取的磺胺类药物进行分析。采用所提出的方法,获得了良好的提取回收率(在五种不同来源的动物组织中为74.0 - 100.3%;n = 3),且基质效应可接受(除肝脏样品外均<10%)。在QuEChERS的净化步骤中,首次使用商用ND-脂质柱从富含脂肪的动物组织中去除疏水性基质成分。此外,使用基质匹配校准(在牛肉中)观察到良好的线性(0.125 - 12.5 ng/g)。牛肉、猪肉和鸡肉样品中的检测限(LOD)估计为0.01 - 0.03 ng/g。对于牛肚和猪肝样品,LOD在0.02 - 0.04 ng/g范围内。使用改进的QuEChERS进行样品前处理,还获得了良好的日内/日间精密度(1.0 - 10.5%/0.4 - 8.0%)和准确度(95.2 - 107.2%/97.8 - 102.1%)。通过测定各种可食用动物组织中目标磺胺类药物的含量,证明了改进的QuEChERS-LC-MS/MS方法在潜在食品安全分析中的适用性。