吡啶离子液体双水相-高效液相色谱法同时测定牛奶中3种喹诺酮药物残留

高等学校化学学报 ›› 2009, Vol. 30 ›› Issue (10): 1956.

吡啶离子液体双水相-高效液相色谱法同时测定牛奶中3种喹诺酮药物残留

曾延波¹, 赵弟海^1,2, 李蕾¹, 王练³, 沈兵³, 奚奇辉³, 张萌萌³

1. 嘉兴学院生物与化学工程学院, 嘉兴 314001;
2. 江西理工大学材料与化学工程学院, 赣州 341000;
3. 嘉兴出入境检验检疫局, 嘉兴 314001

收稿日期:2009-03-09 出版日期:2009-10-10 发布日期:2009-10-10
通讯作者: 李蕾, 男, 教授, 主要从事药物分子识别与分离分析技术研究. E-mail: lileichem@yahoo.com.cn
基金资助:
浙江省科技计划(批准号: 2007C23071, 2007F70011)、浙江省自然科学基金(批准号: Y4080252)和嘉兴市科技计划(批准号: 2008AY2016)资助.

Simultaneous Determination of Three Quionlones Residues in Milk by Pyridinium Ionic Liquid-based Aqueous Two-phase Systems Coupled with High Performance Liquid Chromatography

ZENG Yan-Bo¹, ZHAO Di-Hai^1,2, LI Lei^1*, WANG Lian³, SHEN Bing³, XI Qi-Hui³, ZHANG Meng-Meng³

1. School of Biological and Chemical Engineering, Jiaxing University, Jiaxing 314001, China;
2. School of Material and Chemical Engineering, Jiangxi University of Technology, Ganzhou 341000, China;
3. Jiaxing Entry-Exit Inspection and Quarantine Bureau, Jiaxing 314001, China

Received:2009-03-09 Online:2009-10-10 Published:2009-10-10
Contact: LI Lei. E-mail: lileichem@yahoo.com.cn
Supported by:
浙江省科技计划(批准号: 2007C23071, 2007F70011)、浙江省自然科学基金(批准号: Y4080252)和嘉兴市科技计划(批准号: 2008AY2016)资助.

摘要/Abstract

摘要：

建立了吡啶离子液体双水相-高效液相色谱同时测定牛奶中噁喹酸、萘啶酸及氟甲喹3种喹诺酮药物残留的方法. 牛奶样品经氯化钠和磷酸混合溶液提取后, 采用吡啶离子液体N-乙基-2-甲基吡啶溴化盐([EMPy]Br)和K₂HPO₄形成的双水相体系萃取富集, 以0.1%磷酸水溶液-乙腈为流动相, 梯度洗脱, 紫外检测. 该方法对噁喹酸、萘啶酸和氟甲喹测定的线性范围分别为0.3~15, 0.5~20和0.5~25 μg/mL, 相关系数(r)均大于0.9997, 3种药物的检出限在8~10 μg/kg之间. 对不同加标浓度的牛奶样品测定, 绝对回收率均在86.4%~94.8%范围内, 相对标准偏差为3.6%~8.3%. 该方法对牛奶中喹诺酮药物残留的检测具有简单、快速、环保和灵敏度高等优点.

关键词: 双水相; 吡啶离子液体; 高效液相色谱; 喹诺酮药物检测; 牛奶

Abstract:

A method was developed for the analysis of three quinolones(oxolinic acid, nalidix acid and flumequine) in milk by pyridinium ionic liquid-based aqueous two-phase systems coupled with high performance liquid chromatography. Milk samples were extracted with the mixed solutions consisting of sodium chloride and phosphoric acid. Then extracts were enriched by aqueous two-phase systems composed of the ionic liquid pyridine N-ethyl -2-methyl-pyridine bromide salt([EMPy]Br) and K₂HPO₄. The separation of the analytes was achieved via 0.1% phosphoric acid and acetonitrile with gradient elution under UV detection. The linear ranges are 0.3—15 μg/mL for oxolinic acid, 0.5—20 μg/mL for nalidixic acid and 0.5—25 μg/mL for flumequine. The correlation coefficient(r) is more than 0.9997. The limits of detection are 8—10 μg/kg. Based on detecting spiked quinolones concentrations in milk samples, the absolute recoveries ranged from 86.4% to 94.8% with relative standard deviation from 3.6% to 8.3%. The proposed method of determinating quinolones residues in milk is simple, rapid, friendly to environment and high sensitive.

Key words: Aqueous two-phase systems; Pyridinium ionic liquid; High performance liquid chromatography; Determination of quinolone; Milk

TrendMD:

曾延波, 赵弟海, 李蕾, 王练, 沈兵, 奚奇辉, 张萌萌. 吡啶离子液体双水相-高效液相色谱法同时测定牛奶中3种喹诺酮药物残留. 高等学校化学学报, 2009, 30(10): 1956.

ZENG Yan-Bo, ZHAO Di-Hai, LI Lei*, WANG Lian, SHEN Bing, XI Qi-Hui, .... Simultaneous Determination of Three Quionlones Residues in Milk by Pyridinium Ionic Liquid-based Aqueous Two-phase Systems Coupled with High Performance Liquid Chromatography. Chem. J. Chinese Universities, 2009, 30(10): 1956.

参考文献

[1]Mack G.. J. Chromatogr.
[J], 1992 , 582(122) : 263—266

[2]ZHANG Li-Wei(张黎伟), ZHANG Xin-Xiang(张新祥). Chem. J. Chinese Universities(高等学校化学学报)
[J] , 2008, 29(4): 694—699

[3]Linseman D. A., Hampton L. A., Branstetter D. G.. Fund. Appl. Toxicol.
[J], 1995, 28: 59—64

[4]DING Guo-Hua(丁国华), DING Lei-Ru(丁磊如), LIU Xia(刘霞). Chinese Journal of Hospital Pharm. Acy.(中国医院药学杂志)
[J] , 1995, 8(15) : 380—384

[5]YUE Zhen-Feng(岳振峰), XIE Li-Qi(谢丽琪), CHEN Xiao-Xia(陈小霞), et al.. Journal of Instrumental Analysis(分析测试学报)
[J], 2008, 27(3): 240—243

[6]Ev L. D., Schapoval E. E. S.. J. Pharm. Biomed. Anal.
[J], 2002, 27: 91—96

[7]Khateeb S. Z. E., Razek S. A. A., Amer M. M.. J. Pharm. Biomed. Anal.
[J], 1998, 17: 829—840

[8]Du L. M., Yang Y. Q., Wang Q. M.. Anal. Chim. Acta
[J], 2004, 516: 237—243

[9]Michalska K., Pajchel G., Tyski S.. J. Chromatogr. A
[J], 2004, 1051: 267—272

[10]ZHAO Yan-Yan(赵燕燕), WANG Li-Juan(王丽娟), LI Yue-Qiu(李月秋), et al. . Chem. J. Chinese Universities(高等学校化学学报)
[J] , 2007, 28(1): 62—64

[11]Christodoulou E. A., Samanidou V. F., Papadoyannis I. N.. J. Chromatogr. B
[J], 2007, 859: 246—255

[12]ZHAO Si-Jun(赵思俊), LI Cun(李存), JIANG Hai-Yang(江海洋), et al.. Chinese Journal of Analytical Chemistry(分析化学)
[J], 2007, 35(6): 786—790

[13]Schneider M. J., Donogue D. J.. Anal. Chim. Acta
[J], 2003, 483: 39—49

[14]Chen H. X., Chen H., Jun Y., et al.. Anal. Chim. Acta
[J], 2009, 632: 80—85

[15]Gutowski K. E., Broker G. A., Willauer H. D., et al.. J. Am. Chem. Soc.
[J], 2003, 125: 6632—6633

[16]LIU Qing-Fen(刘庆芬), HU Xue-Sheng(胡雪生), WANG Yu-Hong(王玉红), et al.. Chinese Science Bulletin(科学通报)
[J]. 2005, 50(8): 756—759

[17]DENG Fan-Zheng(邓凡政), GUO Dong-Fang(郭东方). Chinese Journal of Analytical Chemistry(分析化学)
[J], 2006, 34(10): 1451—1453

[18]Li S. H., He C. Y., Liu H. W., et al.. J. Chromatogr. B
[J], 2005, 826: 58—62

[19]He C. Y., Li S. H., Liu H. W., et al.. J. Chromatogr. A
[J], 2005, 1082: 143—149

[20]ZHAO Di-Hai(赵弟海), ZENG Yan-Bo(曾延波), LI Lei(李蕾), et al.. Chinese Journal of Analytical Chemistry(分析化学)
[J], 2009, 37(3): 445—448