超高效液相色谱-质谱联用检测土壤中两种抗生素呋喃唑酮和氟苯尼考

引用本文: 南琼, 唐景春, 何若竹, 胡羽成, 吴涛. 超高效液相色谱-质谱联用检测土壤中两种抗生素呋喃唑酮和氟苯尼考[J]. 分析化学, 2017, 45(11): 1600-1605. doi: 10.11895/j.issn.0253-3820.160870 shu

Citation: NAN Qiong, TANG Jing-Chun, HE Ruo-Zhu, HU Yu-Cheng, WU Tao. Determination of Furazolidone and Florfenicol in Soil by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2017, 45(11): 1600-1605. doi: 10.11895/j.issn.0253-3820.160870 shu

超高效液相色谱-质谱联用检测土壤中两种抗生素呋喃唑酮和氟苯尼考

1.
南开大学环境科学与工程学院, 天津 300071;
2.
环境污染过程与基准教育部重点实验室, 天津 300071;
3.
天津市城市环境污染诊断与修复技术工程中心, 天津 300071;
4.
天津市水利科学研究院, 天津 300061
基金项目:
本文系水体污染控制与治理科技重大专项（No.2015ZX07203-011-06）、天津市水务局局科研项目（No.KY2015-01）和863成果转化项目（No.14RCHZSF00144）资助

摘要: 建立了超高效液相色谱-串联质谱（UPLC/MS/MS）检测土壤中多种环境基质下呋喃唑酮和氟苯尼考的方法。提取液采用磷酸盐缓冲溶液（pH=3）-乙腈（3∶7，V/V），经过SPE固相萃取小柱SAX-HLB串联富集，使用Waters BEH C₁₈色谱柱（2.1×100 mm）进行分离，UPLC/MS/MS在多反应监测模式下进行定性与定量分析。以3倍信噪比确定方法检出限，以10倍信噪比确定方法定量限。结果表明，本方法在5 min内即可分离两种物质，呋喃唑酮和氟苯尼考的检出限分别为1.19和0.41μg/kg；定量限分别为3.40和1.37μg/kg。50μg/L加标水平的呋喃唑酮和氟苯尼考的回收率分别为92%和79%；200μg/L加标水平下呋喃唑酮与氟苯尼考的回收率分别为96%和86%。

关键词:

English

Determination of Furazolidone and Florfenicol in Soil by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

1.
College of Environmental Science and Engineering, Nankai University, Tianjin 300071, China;
2.
Key Laboratory of Pollution Processes and Environmental Criteria, Ministry of Education, Tianjin 300071, China;
3.
Tianjin Engineering Center of Environmental Diagnosis and Contamination Remediation, Tianjin 300071, China;
4.
Tianjin Hydranlic Research Insitute, Tianjin 300061, China
Received Date: 28 November 2016
Revised Date: 04 September 2017

Abstract: A detection method for furazolidone and florfenicol in soil with various environmental matrices was established using ultra performance liquid chromatography-tandem spectrometry (UPLC/MS/MS) technique. Extracting solution of a mixture of phosphate buffer (pH=3) and acetonitrile (3:7, V/V) was used in this experiment. The extracted water samples were enriched by SAX-HLB solid phase extraction column before the process of nitrogen blowing (high purity nitrogen). The enriched antibiotics were desalted with 8 mL of methanol. Waters BEH C₁₈ (2.1×100 mm) column was used for the sample separation. UPLC/MS/MS was carried out for qualitative and quantitative analysis under multi-reaction monitoring mode. The detection limit of the method was determined by 3 times of signal-to-noise ratio, and the limit of determination of the method was determined by 10 times of signal-to-noise ratio. The results showed that the detection limits of furazolidone and florfenicol were 1.19 and 0.41 μg/kg, respectively, and the limits of quantitation of furazolidone and florfenicol were 3.40 and 1.37 μg/kg, respectively. Besides, recovery experiment showed that, for the soil samples spiked with 50 μg/L furazolidone and florfenicol, the recoveries were 79% for florfenicol and 92% for furazolidone. Similarly, for the soil samples spiked with 200 μg/L furazolidone and florfenicol, the recoveries were 96% for furazolidone and 86% for florfenicol.

Key words:

Ultra performance liquid chromatography-tandem spectrometry
/ Furazolidone
/ Florfenicol
/ Solid phase extraction

1. [1]
  Cooper K M, Elliott C T, Kennedyz D G. J. Food Addit. Contam., 2004, 9(21):841-848
2. [2]
  Sai N, Chen Y P, Liu N, Yu G G, Su P, Feng Y, Zhou Z J, Liu X Y, Zhou HY, Gao Z X, Ning B A. Talanta, 2010, 82:1113-1121
3. [3]
  Holt P, Harvey D, Hurley R. Adverse Drug React. Toxicol. Rev., 1993, 12(2):83-89
4. [4]
  Saba A B, Ola-Davies O, Oyeyemi M O, Ajala O.J. Afr. J. Biomed. Res., 2000, 3:133-137
5. [5]
  Wang J, Macneil J D, Kay J F. J. John Wiley & Sons Inc, Hoboken, NJ, USA (2011):121-123
6. [6]
  BangemannM.Cominission Regulation (EC) No 1430/94, Official Journal of the European Cominunities, Brussels, Belgium (1994)
7. [7]
  Ryan J J, Lee Y C, Dupont J A, Charbonneau C F. J. Assoc. Official Anal. Chem., 1975, 58:1227-1238
8. [8]
  Official Methods of Analysis of the Association of Official Analytical Chemists. AOAC Inc., 14th ed., 1984
9. [9]
  Botsoglou N A. J. Agr. Food Chem., 1988, 36(6):1224-1227
10. [10]
  Schering-Plough Animal Health Corporation.Aquafen, AquaflorFlorocol.J. Technical Monograph. New Jersey, USA.http://www.spaquaculture.com/assets/aquaflor, 2003
11. [11]
  NY 5071-2002, The Pollution-free Food Fish with Drug Use. The Ministry of Agriculture of the People's Republic of China. 2002中华人民共和国农业部. 无公害食品渔用药物使用准则NY 5071-2002, 2002
12. [12]
  Saari L, Peltonen K. J. Food Addit. Contam. A, 2004, 21(9):825-832
13. [13]
  Kaniou I, Zachariadis G, Kalligas G, Tsoukali H, Stratis J. J. Liq. Chromatogr., 1994, 17:1385
14. [14]
  Wilhelmus M J, Beek, Marinus M L, Aerts. J. Nucl. Med. Biol., 2017, 44:90-104
15. [15]
  Fernando R, Munasinghe D M S, Gunasena A R C, Abeynayake P. J. Food Control, 2017, 72:300-305
16. [16]
  Cornejo J, Pokrant E, Riquelme R, Briceno C, Maddaleno A, Araya-Jordan C, San M. Food Addit. Contam., 2017, 34(4):469-476
17. [17]
  Lee Y J, Choi J H, Abd El-Aty A M, Chung H S, Lee H S, Kim S W, Rahman M M, Park B J, Kim J E, Shin H C. J. Sep. Sci., 2017, 40(2):415-423
18. [18]
  Orlando E A, Costa R, Aline G, Losekann, Marcos E. J. Chromatogr. B, 2016, 1035:8-15
19. [19]
  XIE Kai-Zhou, XU Dong, CHEN Shu-Qin, XIE Xing, JIA Long-Fei, HUANG Yu-Ping, GUO Hui-Sheng, WANG Jin-Yu, LIU Zong-Ping. Chinese J. Anal. lab., 2011, 30(7):31-35 谢恺舟, 徐东, 陈书琴, 谢星, 贾龙飞, 黄玉萍, 郭辉生, 王金玉, 刘宗平. 分析试验室, 2011, 30(7):31-35
20. [20]
  GUO Xia, ZHANG Su-Xia, SHEN Zhong-Jian, LI Jian-Cheng. Chinese J. CVS., 2006, 9(26):743-747 郭霞, 张素霞, 沈建忠, 李建成. 中国兽医科学, 2006, 36(9):743-747
21. [21]
  Pfenning A P, Roybal J E, Rupp H S. J. AOAC Inter., 1998, 81(4):714
22. [22]
  Tong L, Li P, Wang Y X, Zhu K Z. Chemosphere, 2009, 74(8):1090-1097
23. [23]
  DIAO Shi-Qiang, WU Yan-Yan, LI Lai-Hao, YANG Xian-Qing, SHAO Zheng-Yi, SUN Man-Yi, CHEN Xiao-Feng. Chinese J.Scfs., 2010, 6(2):53-58 刁石强, 吴燕燕, 李来好, 杨贤庆, 邵征翌, 孙满义, 陈晓凤. 南方水产, 2010, 6(2):53-58
24. [24]
  LI Xiao-Jing, HUANG Cong, YU Hong, Zhu Hui-Yang, GAN Ping-Sheng. Chinese J. Env. Health, 2013, 5(30):437-439 李晓晶, 黄聪, 于鸿, 朱惠杨, 甘平胜. 环境与健康杂志, 2013, 30(5):437-439
25. [25]
  MA Li-Li, GUO Chang-Sheng, HU Wei, SHA Jian, ZHU Xing-Wang, RUAN Yue-Pei, WANG Yu-Qiu. Chinese J. Anal. Chem., 2010, 38(1):21-26 马丽丽, 郭昌胜, 胡伟, 沙健, 朱兴旺, 阮悦斐, 王玉秋. 分析化学, 2010, 38(1):21-26
26. [26]
  LI Ling-Ling, HUANG Li-Dong, HUO Jia-Heng, ZHONG Ren-Ci, ZHANG Yong-Song. Chinese J.PNF., 2010, 16(5):1176 -1182 李玲玲, 黄利东, 霍嘉恒, 钟仁赐, 章永松. 植物营养与肥料学报, 2010, 16(5):1176-1182

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沈阳化工大学材料科学与工程学院沈阳 110142

超高效液相色谱-质谱联用检测土壤中两种抗生素呋喃唑酮和氟苯尼考

English

Determination of Furazolidone and Florfenicol in Soil by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

超高效液相色谱-质谱联用检测土壤中两种抗生素呋喃唑酮和氟苯尼考

English

Determination of Furazolidone and Florfenicol in Soil by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

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