分子印迹固相萃取-高效液相色谱法测定饲料中磺胺类药物

引用本文: 杜碧柏, 许杨, 黄运红, 康敏. 分子印迹固相萃取-高效液相色谱法测定饲料中磺胺类药物[J]. 分析化学, 2012, 40(12): 1871-1876. doi: 10.3724/SP.J.1096.2012.20161 shu

Citation: DU Bi-Bai, XU Yang, Huang Yun-Hong, Kang Min. Determination of Sulfonamides in Feeds by High Performance Liquid Chromatography with Molecularly Imprinted Solid Phase Extraction[J]. Chinese Journal of Analytical Chemistry, 2012, 40(12): 1871-1876. doi: 10.3724/SP.J.1096.2012.20161 shu

分子印迹固相萃取-高效液相色谱法测定饲料中磺胺类药物

杜碧柏 ^1, ,
许杨 ^, ,
黄运红 ^1,2, ,
康敏 ^1,

通讯作者: 许杨

基金项目:
本文系食品科学与技术国家重点实验室自由探索课题(No.SKLF-TS-200815)资助 (No.SKLF-TS-200815)

摘要: 建立了基于分子印迹聚合物(MIPs)为吸附剂的固相萃取技术结合高效液相色谱检测饲料中5种磺胺类药物(SAs)的方法。以磺胺嘧啶为模板,采用紫外光引发合成MIPs,以MIPs作为吸附剂制备固相萃取柱,并对上柱、淋洗和洗脱等萃取条件进行了优化。在优化的条件下,5种SAs的检出限为0.14-0.23 mg/kg;定量限为0.38-0.47 mg/kg;平均回收率在72.1%-89.3%之间;批内与批间相对标准偏差分别小于7.9%和9.2%。与碱性氧化铝柱净化相比,分子印迹固相萃取柱净化后杂质更少,选择性更好,方法的定量限更低。

关键词:

English

Determination of Sulfonamides in Feeds by High Performance Liquid Chromatography with Molecularly Imprinted Solid Phase Extraction

1.
¹ State Key Laboratory of Food Science and Technology, Sino-Germany Joint Research Institute, Nanchang University, Nanchang 330047, China;

Corresponding author: 许杨

Received Date: 22 February 2012
Fund Project:
本文系食品科学与技术国家重点实验室自由探索课题(No.SKLF-TS-200815)资助

Abstract: A method was developed for monitoring five sulfonamides (SAs) in feeds by using molecularly imprinted polymers (MIPs) as selective solid-phase extraction sorbents coupled with high performance liquid chromatography. The MIPs were firstly synthesized by ultraviolet initiated using sulfadiazine as template. Then, the molecularly printed solid phase extraction (MISPE) column was prepared, and the MIPs were used as adsorbent. Meanwhile, the procedures of loading, washing and eluting conditions were optimized. Under the optimum conditions, the detection limit range of five SAs was 0.14-0.23 mg/kg and the quantification limit range was 0.38-0.47 mg/kg. The average recoveries were in the range of 72.1%-89.3% with a batch and batch sampling relative standard deviations less than 7.9% and 9.2%, respectively. It showed that the MISPE column decreased the matrix effect and had a better selectivity and a lower limit of quantification than Alumina B column.

Key words:

Molecularly imprinted polymer
/ Solid-phase extraction
/ Sulfonamides
/ Feed
/ High performance liquid chromatography

1. [1]
  1 Heuer H, Solehati Q, Zimmerling U, Kleineidam K, Schloter M, Müller T, Focks A, Thiele-Bruhn S, Smalla K. Appl. Environ. Microb., 2011, 77(7): 2527-25301 Heuer H, Solehati Q, Zimmerling U, Kleineidam K, Schloter M, Müller T, Focks A, Thiele-Bruhn S, Smalla K. Appl. Environ. Microb., 2011, 77(7): 2527-2530
2. [2]
  2 Willmott A, McCombie A, Rossleigh M. Intern. Med. J., 2011, 41(Suppl. 3): 25-262 Willmott A, McCombie A, Rossleigh M. Intern. Med. J., 2011, 41(Suppl. 3): 25-26
3. [3]
  3 Wang S, Zhang H Y, Wang L, Duan Z J, Kennedy I. Food Addit. Contam., 2006, 23(4): 362-3843 Wang S, Zhang H Y, Wang L, Duan Z J, Kennedy I. Food Addit. Contam., 2006, 23(4): 362-384
4. [4]
  4 LIU Gui-Hua, HAN De-Man, Liang Hua-Ding, TANG Shou-Wan, PAN Fu-You, YAN Rui-Qiang. Chinese J. Anal. Chem., 2012, 40(3): 432-4364 LIU Gui-Hua, HAN De-Man, Liang Hua-Ding, TANG Shou-Wan, PAN Fu-You, YAN Rui-Qiang. Chinese J. Anal. Chem., 2012, 40(3): 432-436
5. [5]
  刘贵花, 韩德满, 梁华定, 唐守万, 潘富友, 阎瑞强. 分析化学, 2012, 40(3): 432-436刘贵花, 韩德满, 梁华定, 唐守万, 潘富友, 阎瑞强. 分析化学, 2012, 40(3): 432-436
6. [6]
  5 Blüthgen A H. Bull. Int. Dairy Feder., 2000, 356: 43-475 Blüthgen A H. Bull. Int. Dairy Feder., 2000, 356: 43-47
7. [7]
  6 Segato G, Benetti C, Angeletti R, Montesissa C, Biancotto G. Food Addit. Contam. A, 2011, 28(7): 860-8686 Segato G, Benetti C, Angeletti R, Montesissa C, Biancotto G. Food Addit. Contam. A, 2011, 28(7): 860-868
8. [8]
  7 Albert K, Riter K L, Smallidge R L. J. Aoac Int , 2003, 86(4): 623-6307 Albert K, Riter K L, Smallidge R L. J. Aoac Int , 2003, 86(4): 623-630
9. [9]
  8 Iammarino M, Palermo C, Nardiello D, Muscarella M. Chromatographia, 2011, 73(Suppl. 1): S75-S828 Iammarino M, Palermo C, Nardiello D, Muscarella M. Chromatographia, 2011, 73(Suppl. 1): S75-S82
10. [10]
  9 Borràs S, Companyó R, Guiteras J. J. Agr. Food Chem., 2011, 59(10): 5240-52479 Borràs S, Companyó R, Guiteras J. J. Agr. Food Chem., 2011, 59(10): 5240-5247
11. [11]
  10 Kumar P, Companyó R. Drug Test. Anal, 2012, 4(5): 368-37510 Kumar P, Companyó R. Drug Test. Anal, 2012, 4(5): 368-375
12. [12]
  11 Croubels S, Wassink P, de Backer P. Anal. Chim. Acta, 2002, 473(1-2): 183-19411 Croubels S, Wassink P, de Backer P. Anal. Chim. Acta, 2002, 473(1-2): 183-194
13. [13]
  12 Kantiani L, Farré M, Freixiedas J M G I, Barceló D. J. Chromatogr. A, 2010, 1217(26): 4247-425412 Kantiani L, Farré M, Freixiedas J M G I, Barceló D. J. Chromatogr. A, 2010, 1217(26): 4247-4254
14. [14]
  13 Liu R Y, He P L, Li Z, Li R G. J. Chromatogr. Sci., 2011, 49(8): 640-64613 Liu R Y, He P L, Li Z, Li R G. J. Chromatogr. Sci., 2011, 49(8): 640-646
15. [15]
  14 HU Xiao-Gang, LI Gong-Ke. Chinese J. Anal. Chem., 2006, 34(7): 1035-104114 HU Xiao-Gang, LI Gong-Ke. Chinese J. Anal. Chem., 2006, 34(7): 1035-1041
16. [16]
  胡小刚, 李攻科. 分析化学, 2006, 34(7): 1035-1041胡小刚, 李攻科. 分析化学, 2006, 34(7): 1035-1041
17. [17]
  15 YAN Hong-Yuan, YANG Geng-Liang. Chinese J. Chromatogr., 2011, 29(7): 572-57915 YAN Hong-Yuan, YANG Geng-Liang. Chinese J. Chromatogr., 2011, 29(7): 572-579
18. [18]
  闫宏远, 杨更亮. 色谱, 2011, 29(7): 572-579闫宏远, 杨更亮. 色谱, 2011, 29(7): 572-579
19. [19]
  16 Guo L Y, Jiang X M, Yang C L, Zhang H X. Anal. Bioanal. Chem., 2008, 391(6): 2291-229816 Guo L Y, Jiang X M, Yang C L, Zhang H X. Anal. Bioanal. Chem., 2008, 391(6): 2291-2298
20. [20]
  17 He J X, Wang S, Fang G Z, Zhu H P, Zhang Y. J. Agric. Food Chem., 2008, 56(9): 2919-292517 He J X, Wang S, Fang G Z, Zhu H P, Zhang Y. J. Agric. Food Chem., 2008, 56(9): 2919-2925
21. [21]
  18 Vlatakis G, Andersson L I, Müller R, Mosbach K. Nature, 1993, 361(6413): 645-64718 Vlatakis G, Andersson L I, Müller R, Mosbach K. Nature, 1993, 361(6413): 645-647
22. [22]
  19 Zhou X, He X W, Chen L X, Li W Y, Zhang Y K. Chinese J. Anal. Chem., 2009, 37(2): 174-18019 Zhou X, He X W, Chen L X, Li W Y, Zhang Y K. Chinese J. Anal. Chem., 2009, 37(2): 174-180
23. [23]
  周雪, 何锡文, 陈朗星, 李文友, 张玉奎. 分析化学, 2009, 37(2): 174-180周雪, 何锡文, 陈朗星, 李文友, 张玉奎. 分析化学, 2009, 37(2): 174-180
24. [24]
  20 LIU Hui-Jun, XU Wei-Jian, LIU Yao-Chi, XIONG Yuan-Qin. Spectrosc. Spect. Anal., 2007, 27(8): 1596-159920 LIU Hui-Jun, XU Wei-Jian, LIU Yao-Chi, XIONG Yuan-Qin. Spectrosc. Spect. Anal., 2007, 27(8): 1596-1599
25. [25]
  刘慧君, 徐伟箭, 刘耀驰, 熊远钦. 光谱与光谱分析, 2007, 27(8): 1596-1599刘慧君, 徐伟箭, 刘耀驰, 熊远钦. 光谱与光谱分析, 2007, 27(8): 1596-1599
26. [26]
  21 Zheng N, Li Y Z, Chang W B, Wang Z M, Li T J. Anal. Chim. Acta., 2002, 452(2): 277-28321 Zheng N, Li Y Z, Chang W B, Wang Z M, Li T J. Anal. Chim. Acta., 2002, 452(2): 277-283
27. [27]
  22 ZHANG Feng, XU Cheng-Bao, LAN Fang, WANG Xiu-Juan, YONG Wei , SUO Ruan, CHU Xiao-Gang , DING Fei , LV Quan-Fu . Chinese J. Anal. Chem., 2012, 40(1): 101-10622 ZHANG Feng, XU Cheng-Bao, LAN Fang, WANG Xiu-Juan, YONG Wei , SUO Ruan, CHU Xiao-Gang , DING Fei , LV Quan-Fu . Chinese J. Anal. Chem., 2012, 40(1): 101-106
28. [28]
  张峰, 许成保, 蓝芳, 王秀娟, 雍炜, 锁然, 储晓刚, 丁菲, 吕泉福. 分析化学, 2012, 40(1): 101-106张峰, 许成保, 蓝芳, 王秀娟, 雍炜, 锁然, 储晓刚, 丁菲, 吕泉福. 分析化学, 2012, 40(1): 101-106
29. [29]
  23 GB/T 19542-2007. Determination of Sulfonamides in Feeds-High Performance Liquid Chromatography. National Standards of the People's Republic of China23 GB/T 19542-2007. Determination of Sulfonamides in Feeds-High Performance Liquid Chromatography. National Standards of the People's Republic of China
30. [30]
  GB/T 19542-2007. 饲料中磺胺类药物的测定-高效液相色谱法. 中华人民共和国国家标准GB/T 19542-2007. 饲料中磺胺类药物的测定-高效液相色谱法. 中华人民共和国国家标准

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

分子印迹固相萃取-高效液相色谱法测定饲料中磺胺类药物

通讯作者: 许杨

English

Determination of Sulfonamides in Feeds by High Performance Liquid Chromatography with Molecularly Imprinted Solid Phase Extraction

Corresponding author: 许杨

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

分子印迹固相萃取-高效液相色谱法测定饲料中磺胺类药物

通讯作者: 许杨

English

Determination of Sulfonamides in Feeds by High Performance Liquid Chromatography with Molecularly Imprinted Solid Phase Extraction

Corresponding author: 许杨

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

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

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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