Abstract
Based on solid phase extraction (SPE) and ultra high performance liquid chromatography (UPLC) technique, a method has been developed for the simultaneous detection and analysis of 6 fluoroquinolones residues in aquatic products. The optimized process and parameters of this method were as followed: treated aquatic products were extracted with phosphate buffer, the extracting solution were purified by SPE and concentrated by blowing nitrogen, and the residues were then dissolved in 0.2% formic acid solution for UPLC analysis; Chromatographic column BEH C18 (1.7 μm, 2.1 mm×50 mm) were applied, and citric acid (0.05 mol/L)-ammonium acetate (0.1 mol/L) buffer were used as the mobile phase with 0.42 mL/min. the sample volume was 0.2 μL, column temperature was 50 degree centigrade, and the excitation and emission wave length of fluorescence detector were 278 nm and 465 nm, respectively. The proposed method is simple and effective, with recovery rate range between 63.69% and 90.83%, limit of detection range between 0.5 and 1.8 μg/kg, and relative standard deviation less than 10%.
Publication Date
5-28-2018
First Page
77
Last Page
81
DOI
10.13652/j.issn.1003-5788.2018.05.015
Recommended Citation
Jiang, HE; Xiaoyue, LI; Yujie, QIU; Boen, LI; and Pinhong, YANG
(2018)
"Determination of 6 fluoroquinolones residues in aquatic products by solid phase extraction and ultra performance lquid chromatography,"
Food and Machinery: Vol. 34:
Iss.
5, Article 15.
DOI: 10.13652/j.issn.1003-5788.2018.05.015
Available at:
https://www.ifoodmm.cn/journal/vol34/iss5/15
References
[1] 丑亚琴, 唐巍, 卢艳芬, 等. 高效液相色谱法同时测定水产品中四种氟喹诺酮类药物残留前处理条件的优化[J]. 水产养殖, 2013(1): 21-27.
[2] DRLICA K, MALIK M, KERNS R J. Quinolone-mediated bacterial death [J]. Antimicrobial Agents and Chemotherapy, 2008, 52(2): 385-392.
[3] 钱卓真, 苏秀华, 魏博娟, 等. 高效液相色谱法同时测定水产品中6种喹诺酮药物的残留[J]. 食品科学, 2010, 31(6): 185-189.
[4] 陈佳虹. 喹诺酮类药物广谱免疫分析研究[D]. 广州: 华南农业大学, 2016: 1-3.
[5] 彭娟. 三类重要渔药残留免疫快速检测技术[D]. 无锡: 江南大学, 2017: 10-13.
[6] IBARRA I S, RODRLGUEZ J A, PAEZ-HERNANDEZ M E, et al. Determination of quinolones in milk samples using a combination of magnetic solid-phase extraction and capillary electrophoresis[J]. Electrophoresis, 2012, 33(7): 2 041-2 048.
[7] 张玉洁, 李倩, 汪霞, 等. 高效液相色谱法检测多种动物组织中氟喹诺酮类药物残留量的研究[J]. 中国兽药杂志, 2012, 46(7): 18-22.
[8] 李佩佩, 张小军, 张帅, 等. 通过式固相萃取结合超高效液相色谱-四级杆飞行时间质谱筛查鱼肉中多类兽药残留[J]. 浙江海洋学院学报: 自然科学版, 2017, 36(3): 228-234.
[9] BABIC S, PAVLOVIC D M, ASPERGE D, et al. Determination of multi-class pharmaceuticals in wastewater by liquid chromatography-tandem mass spectrometry(LC-MS-MS)[J]. Analytical and Bioanalytical Chemistry, 2010, 398(3): 1 185-1 194.
[10] PASCHOAL J A, REYES F G, RATH S. Quantitation and identity confirmation of residues of quinolones in tilapia fillets by LC-ESI-MS-MS QToF[J]. Analytical and Bioanalytical Chemistry, 2009, 394(8): 2 213-2 221.
[11] 惠芸华, 张晓玲, 金高娃, 等. 高效液相色谱法测定水产品中9种氟喹诺酮类药物残留[J]. 海洋渔业, 2010, 32(2): 204-210.
[12] 丑亚琴, 唐巍, 卢艳芬, 等. 高效液相色谱法同时测定水产品中四种氟喹诺酮类药物残留前处理条件的优化[J]. 水产养殖, 2013, 34(1): 21-27.
[13] 王志杰, 冷凯良, 孙伟红, 等. 高效液相色谱-串联质谱内标法同时测定水产品中15种喹酮类药物残留量[J]. 分析科学学报, 2010, 26(4): 409-414.
[14] 钱卓真, 苏秀华, 魏博娟, 等. 高效液相色谱法同时测定水产品中6种喹诺酮药物的残留[J]. 食品科学, 2010, 31(6): 185-189.
[15] Wisconsin Department of Natural Resources Laboratory Certification Program. Analytical Detection Limit Guidance & Laboratory Guide for Determining Method Detection Limits: PUBL-TS-056-96 [S/OL]. [2017-10-26]. https://dnr.wi.gov/Regulations/labCert/documents/guidance/-LODguide.pdf.
[16] 王丽娟, 张骊, 钱卓真, 等. 液相色谱检测水产品中喹诺酮类药物的方法改进研究[J]. 中国兽药杂志, 2015, 49(5): 37-42.
[17] 惠芸华, 沈晓盛, 冯兵, 等. 固相萃取-高效液相色谱法测定水产品中7种氟喹诺酮类药物残留[J]. 农药学学报, 2009, 11(4): 462-466.
[18] 汤轶伟, 孙征, 沙莎, 等. 水产品中恩诺沙星药物残留检测方法研究进展[J]. 渤海大学学报: 自然科学版, 2014, 35(1): 77-83.
[19] CAADACAADA F, ESPINOSAMANSILLA A, JIMNEZ GIRN A, et al. Simultaneous determination of the residues of fourteen quinolones and fluoroquinolones in fish samples using liquid chromatography with photometric and fluorescence detection[J]. Czech Journal of Food Sciences, 2012, 30(1): 74-82.