磁性多壁碳纳米管净化技术快速测定水中多种抗生素残留
Quick Determination of Antibiotics Residues in Water Samples by Magnetic Multiwalled Carbon Nanotubes Cleaning Technology

DOI: 10.12677/AAC.2016.64015, PP. 96-104

Keywords: 超高效液相色谱-串联质谱，磁性多壁碳纳米管，抗生素，残留
Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry, Magnetic Multiwalled Carbon Nanotubes, Antibiotics, Residues

Full-Text   Cite this paper   Add to My Lib

Abstract:

采用磁性多壁碳纳米管-超高效液相色谱/质谱/质谱(UPLC/MS/MS)技术测定水样中23种抗生素残留量。水样基质中的23种抗生素药物先采用磁性多壁碳纳米管(MWCNTs)富集和净化，再用5%的氨水甲醇溶液脱附，23种化合物以CORTECS^TM C₁₈₊色谱柱分离，甲醇和0.1%的甲酸水溶液作为流动相，采用电喷雾正离子(ESI+)和多反应监测模式(MRM)分析，外标法定量。23种抗生素在0.5~50 μg/L的浓度范围内线性相关系数均大于0.99，检出限为0.01 μg/L，定量限为0.03 μg/L。在0.05、0.5、10 μg/L不同浓度水平下，23种抗生素的平均回收率在87.5%~105.8%之间，相对标准偏差在0.3%~4.2%之间。由于该技术简便、快速、灵敏度高，适用于水中23种抗生素残留的快速测定。
A method was established for determining 23 antibiotics residues in water samples by magnetic multiwalled carbon nanotubes and ultra performance liquid chromatography-tandem mass spectrometry (UPLC/MS/MS). The 23 antibiotics in water samples were first enriched and cleaned up by magnetic multiwalled carbon nanotubes, and then eluted with ammonium hy-droxide-methanol (5:95, v/v). The target antibiotics were separated by Waters CORTECS^TM C₁₈₊ column using methanol and 0.1% formate in water as mobile phases. The analytes were detected by positive electrospray ionization with multiple reaction monitoring. External standard method was used to determine the quantity. In the linear range of 0.5~50 μg/L, the correlation coefficients of 23 antibiotics were greater than 0.99, the limit of detection (LOD) was 0.01 μg/L, and the limit of quantitation (LOQ) was 0.03 μg/L. The mean recoveries at the three spiked levels of 0.05, 0.5, 10 μg/L were 87.5%~105.8%. The relative standard deviation (RSD) was 0.3%~4.2%. The simplicity, sensitivity and good precision of the method made it be well suitable for quick determination of the 23 antibiotics residues in water samples.

References

[1]	Jouzel, J.N. and Prete, G. (2016) Becoming a Victim of Pesticides: Legal Action and Its Effects on the Mobilization of Affected Farmworkers. Sociologie Du Travail, 57, E63-E80. http://dx.doi.org/10.1016/j.soctra.2015.09.010
[2]	Houbraken, M., Spranghers, T., De Clercq, P., et al. (2016) Pesticide Contamination of Tenebrio molitor (Coleoptera: Tenebrionidae) for Human Consumption. Food Chemistry, 201, 264-269. http://dx.doi.org/10.1016/j.foodchem.2016.01.097
[3]	Hong, J., Kawashima, A., Okamoto, M., Kanetsuki, K., Makino, T. and Hamada, N. (2016) Fundamental Study of a Novel Membrane Filtration Cleanup Method for Pesticide Analysis in Agricultural Products. Food Control, 64, 1-9. http://dx.doi.org/10.1016/j.foodcont.2015.12.003
[4]	Rizzetti, T.M., Kemmerich, M.L., Martins, L., Prestes, O.D., Adaime, M.B. and Zanella, R. (2016) Optimization of a QuEChERS Based Method by Means of Central Composite Design for Pesticide Mul-tiresidue Determination in Orange Juice by UHPLC-MS/MS. Food Chemistry, 196, 25-33. http://dx.doi.org/10.1016/j.foodchem.2015.09.010
[5]	Hou, F., Zhao, L.W. and Liu, F.M. (2016) Determination of Chloro-thalonil Residue in Cabbage by a Modified QuEChERS-Based Extraction and Gas Chromatography-Mass Spectrometry. Food Ana-lytical Methods, 9, 656-663. http://dx.doi.org/10.1007/s12161-015-0228-1
[6]	Grande-Martinez, A., Arrebola-Liebanas, F.J., Martinez-Vidal, J.L., Her-nández-Torres, M.E. and Garrido-Frenich, A. (2016) Optimization and Validation of a Multiresidue Pesticide Method in Rice and Wheat Flour by Modified QuEChERS and GC-MS/MS. Food Analytical Methods, 9, 548-563. http://dx.doi.org/10.1007/s12161-015-0214-7
[7]	高立红, 史亚利, 厉文辉, 等. 高效液相色谱-电喷雾串联质谱法检测环境水样中22种抗生素类药物[J]. 色谱, 2010, 28(5): 491-497.
[8]	尹燕敏, 沈颖青, 顾海东, 等. 固相萃取-液质联用法同时测定水中的喹诺酮类和磺胺类抗生素[J]. 化学分析计量, 2013, 22(3): 29-32.
[9]	雷晓宁, 鲁建江, 刘子龙, 等. 高效液相色谱-电喷雾串联质谱法同步检测污水处理厂活性污泥中12种抗生素[J]. 石河子大学学报(自然科学版), 2013, 31(6): 759-764.
[10]	Zhao, Q., Wei, F., Luo, Y.B., Ding, J., Xiao, N. and Feng, Y.-Q. (2011) Rapid Magnetic Solid-Phase Extraction Based on Magnetic Multiwalled Carbon Nanotubes for the Determination of Polycyclic Aromatic Hydrocarbons in Edible Oils. Journal of Agricultural and Food Chemistry, 59, 12794-12800. http://dx.doi.org/10.1021/jf203973s
[11]	Xu, Y., Ding, J., Chen, H.Y., et al. (2013) Fast Determination of Sulfonamides from Egg Samples Using Magnetic Multiwalled Carbon Nanotubes as Adsorbents Followed By Liquid Chromatography-Tandem Mass Spectrometry. Food Chemistry, 140, 83-90. http://dx.doi.org/10.1016/j.foodchem.2013.02.078
[12]	曹慧, 陈小珍, 朱岩, 等. 磁性多壁碳纳米管对磺胺类药物的吸附行为[J]. 新型炭材料, 2015, 30(6): 572-578.

Full-Text