分子印迹固相萃取-超高效液相色谱-串联质谱法快速测定猪尿中15种<i>β</i><sub>2</sub>-受体激动剂残留

引用本文: 王丽君, 曹旭敏, 孙晓亮, 王淑婷, 刘静, 郝智慧, 曲宝涵, 赵思俊. 分子印迹固相萃取-超高效液相色谱-串联质谱法快速测定猪尿中15种β₂-受体激动剂残留[J]. 色谱, 2016, 34(3): 240-248. doi: 10.3724/SP.J.1123.2015.11003 shu

Citation: WANG Lijun, CAO Xumin, SUN Xiaoliang, WANG Shuting, LIU Jing, HAO Zhihui, QU Baohan, ZHAO Sijun. Rapid determination of 15 β ₂-agonists residues in swine urine by ultra performance liquid chromatography-tandem mass spectrometry coupled with molecularly imprinted solid phase extraction[J]. Chinese Journal of Chromatography, 2016, 34(3): 240-248. doi: 10.3724/SP.J.1123.2015.11003 shu

分子印迹固相萃取-超高效液相色谱-串联质谱法快速测定猪尿中15种β₂-受体激动剂残留

王丽君 ^1,2,3, ,
曹旭敏 ^2,3, ,
孙晓亮 ^2,3, ,
王淑婷 ^2,3, ,
刘静 ^2, ,
郝智慧 ^1, ,
曲宝涵 ^{1,
,} ,
赵思俊 ^{2,3,
,}

1.
1. 青岛农业大学化学与药学院, 山东青岛 266109;
2.
2. 中国动物卫生与流行病学中心动物产品安全监测室, 山东青岛 266032;
3.
3. 农业部畜禽产品质量安全风险评估实验室(青岛), 山东青岛 266032

通讯作者: 曲宝涵,赵思俊; 曲宝涵,赵思俊

基金项目:
国家畜禽质量安全风险评估项目(GJFP2015007) (GJFP2015007)

中国动物卫生与流行病学中心创新基金项目(2014IF-0003FF). (2014IF-0003FF)

摘要: 建立了分子印迹固相萃取(MISPE)-超高效液相色谱-串联质谱(UPLC-MS/MS)快速测定猪尿中15种 β ₂-受体激动剂的分析方法。分别优化了上样溶液的pH值、淋洗和洗脱溶液等MISPE净化条件及质谱条件。将猪尿样品离心,经MISPE柱上样,依次用水、乙腈、0.5%(v/v)乙酸乙腈溶液淋洗,10%(v/v)乙酸甲醇溶液洗脱,氮气吹干,0.1%(v/v)甲酸水-乙腈(9 : 1, v/v)复溶;采用BEH C₁₈色谱柱分离,以乙腈-0.1%(v/v)甲酸水溶液为流动相,采用梯度洗脱,在电喷雾正离子多反应监测模式下外标法定量。考察了MISPE对15种 β ₂-受体激动剂的吸附特异性;猪尿中15种 β ₂-受体激动剂在0.1~20 μ g/L范围内线性关系良好(r²≥0.992);检出限和定量限分别为0.03和0.1 μ g/L; 15种 β ₂-受体激动剂的加标回收率为65.6%~115.0%,批内、批间相对标准偏差分别为0.57%~16.1%和1.11%~16.8%。该方法操作简单、快速、灵敏度高、特异性好。

关键词:

English

Rapid determination of 15 β ₂-agonists residues in swine urine by ultra performance liquid chromatography-tandem mass spectrometry coupled with molecularly imprinted solid phase extraction

1.
1. School of Chemistry and Pharmaceutical Sciences, Qingdao Agricultural University, Qingdao 266109, China;
2.
2. Department for Safety Supervision of Animal Products, China Animal Health and Epidemiology Center, Qingdao 266032, China;
3.
3. Livestock and Poultry Products Quality and Safety Risk Assessment Laboratory, Ministry of Agriculture (Qingdao), Qingdao 266032, China

Corresponding author: 曲宝涵,赵思俊; 曲宝涵,赵思俊

Received Date: 02 November 2015
Fund Project:
国家畜禽质量安全风险评估项目(GJFP2015007)

中国动物卫生与流行病学中心创新基金项目(2014IF-0003FF).

Abstract: An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method coupled with molecularly imprinted solid phase extraction (MISPE) for rapid determination of 15 β ₂-agonists residues in swine urine has been established. In order to obtain the optimized purification conditions, different pH values of loading, washing and elution solvents for the MISPE procedure were optimized. Finally, the swine urine samples (pH 7.0) were performed directly by MISPE column, then the column was washed with water, acetonitrile and 0.5%(v/v) acetic acid in acetonitrile, and eluted with 10%(v/v) acetic acid in methanol. Meanwhile, the parameters of UPLC-MS/MS have been optimized.The UPLC separation was performed on a BEH C₁₈ column, and eluted with the mobile phase consisting of 0.1%(v/v) formic acid aqueous solution and acetonitrile with linear gradient program. The analysis was in ESI positive ion scan mode and multiple reaction monitoring (MRM) mode. Under the optimum conditions, the blank swine urine was spiked with different concentrations analytes and taken for analysis to evaluate the established method. To highlight the advantage of MISPE, specificity adsorption for the 15 β ₂-agonists in swine urine was investigate. The linear ranges were 0.1-20 μ g/L for the 15 β ₂-agonists ( r ²≥0.992). The limits of detection (LODs) and the limits of quantification (LOQs) were 0.03 and 0.1 μ g/L, respectively. At the spiked levels of 0.1, 0.5 and 2.5 μ g/L in blank samples, the mean recoveries were 65.6%-115.0% with the relative standard deviations (RSDs, n=6) of 0.57%-16.1%. Overall, the proposed method is simple, quick, reliable,sensitive, and can be applied in large scale supervision of illegal usage of the 15 β ₂-agonists.

Key words:

1. [1] Yan H, Xu D, Meng H, et al. Qual AssurSaf Crop, 2015, 7(1): 27 [1] Yan H, Xu D, Meng H, et al. Qual AssurSaf Crop, 2015, 7(1): 27
2. [2] Barbosa J, Cruz C, Martins J, et al. Food Addit Contam, 2005, 22(6): 563 [2] Barbosa J, Cruz C, Martins J, et al. Food Addit Contam, 2005, 22(6): 563
3. [3] Fredy M T, Salvador V L, Arturo E M, et al. J Food Drug Anal, 2013, 21(4): 414 [3] Fredy M T, Salvador V L, Arturo E M, et al. J Food Drug Anal, 2013, 21(4): 414
4. [4] Nie J R, Zhu M L, Lian J, et al. Chinese Journal of Chromatography, 2010, 28(8): 759 聂建荣, 朱铭立, 连槿, 等. 色谱, 2010, 28(8): 759 [4] Nie J R, Zhu M L, Lian J, et al. Chinese Journal of Chromatography, 2010, 28(8): 759 聂建荣, 朱铭立, 连槿, 等. 色谱, 2010, 28(8): 759
5. [5] Meng W Y, Guo Z M, Shen W J, et al. Chinese Journal of Chromatography, 2012, 30(2): 141 孟文瑛, 郭志谋, 沈伟健, 等. 色谱, 2012, 30(2): 141[5] Meng W Y, Guo Z M, Shen W J, et al. Chinese Journal of Chromatography, 2012, 30(2): 141 孟文瑛, 郭志谋, 沈伟健, 等. 色谱, 2012, 30(2): 141
6. [6] Zheng L, Wu Y J, Zhao Y F, et al. Chinese Journal of Chromatography, 2014, 32(8): 867 郑玲, 吴玉杰, 赵永峰, 等. 色谱, 2014, 32(8): 867 [6] Zheng L, Wu Y J, Zhao Y F, et al. Chinese Journal of Chromatography, 2014, 32(8): 867 郑玲, 吴玉杰, 赵永峰, 等. 色谱, 2014, 32(8): 867
7. [7] Du X D, Wu Y L, Yang H J, et al. J Chromatogr A, 2012, 1260: 25 [7] Du X D, Wu Y L, Yang H J, et al. J Chromatogr A, 2012, 1260: 25
8. [8] Liu W, Yan Z M, Huang X Y, et al. Talanta, 2015, 132: 915 [8] Liu W, Yan Z M, Huang X Y, et al. Talanta, 2015, 132: 915
9. [9] Liu W, Zhang L, Wei Z Y, et al. J Chromatogr A, 2009, 1216: 5340 [9] Liu W, Zhang L, Wei Z Y, et al. J Chromatogr A, 2009, 1216: 5340
10. [10] Wang D, Yang S M, Liu X W, et al. Chinese Journal of Instrumental Analysis, 2010, 29(8): 812 王迪, 杨曙明, 刘潇威, 等. 分析测试学报, 2010, 29(8): 812[10] Wang D, Yang S M, Liu X W, et al. Chinese Journal of Instrumental Analysis, 2010, 29(8): 812 王迪, 杨曙明, 刘潇威, 等. 分析测试学报, 2010, 29(8): 812
11. [11] Huang Y, Zhang Q J, Liu M, et al. Chinese Journal of Chromatography, 2012, 30(1): 56 黄怡, 张青杰, 刘敏, 等. 色谱, 2012, 30(1): 56[11] Huang Y, Zhang Q J, Liu M, et al. Chinese Journal of Chromatography, 2012, 30(1): 56 黄怡, 张青杰, 刘敏, 等. 色谱, 2012, 30(1): 56
12. [12] Yan H Y, Liu S T, Gao M M, et al. J Chromatogr A, 2013, 1294: 10 [12] Yan H Y, Liu S T, Gao M M, et al. J Chromatogr A, 2013, 1294: 10
13. [13] Du W, Lei C M, Zhang S R, et al. J Pharm Biomed Anal, 2014, 91: 160 [13] Du W, Lei C M, Zhang S R, et al. J Pharm Biomed Anal, 2014, 91: 160
14. [14] Lei Y, Xu G H, Wei F D, et al. J Pharm Biomed Anal, 2014, 94: 118 [14] Lei Y, Xu G H, Wei F D, et al. J Pharm Biomed Anal, 2014, 94: 118
15. [15] Zhang X L, Luo Y J, Jiang J, et al. Chinese Journal of Chromatography, 2015, 33(8): 838 张学亮, 罗云敬, 姜洁, 等. 色谱, 2015, 33(8): 838 [15] Zhang X L, Luo Y J, Jiang J, et al. Chinese Journal of Chromatography, 2015, 33(8): 838 张学亮, 罗云敬, 姜洁, 等. 色谱, 2015, 33(8): 838
16. [16] Gholivand M B, Khodadadian M, Ahmadi F. Anal Chim Acta, 2010, 658(2): 225 [16] Gholivand M B, Khodadadian M, Ahmadi F. Anal Chim Acta, 2010, 658(2): 225
17. [17] Martín-Esteban A. Trend Anal Chem, 2013, 45: 169 [17] Martín-Esteban A. Trend Anal Chem, 2013, 45: 169
18. [18] Ansell R J. Adv Drug Deliv Rev, 2005, 57(12): 1809 [18] Ansell R J. Adv Drug Deliv Rev, 2005, 57(12): 1809
19. [19] Gros M, Pizzolato T M, Petrovic M, et al. J Chromatogr A, 2008, 1189: 374 [19] Gros M, Pizzolato T M, Petrovic M, et al. J Chromatogr A, 2008, 1189: 374
20. [20] Wang P L. [MS Dissertation]. Beijing: Chinese Academy of Agricultural Sciences, 2012 王培龙. [硕士学位论文]. 北京: 中国农业科学院, 2012[20] Wang P L. [MS Dissertation]. Beijing: Chinese Academy of Agricultural Sciences, 2012 王培龙. [硕士学位论文]. 北京: 中国农业科学院, 2012
21. [21] Ministry of Agriculture. No. 1025-11 Bulletin of the Ministry of Agriculture of the People's Republic of China. (2008-04-29)[2015-02-10]. http://www.docin.com/p-1062235395.html 农业部.中华人民共和国农业部公告第1025-11号. (2008-04-29)[2015-02-10]. http://www.docin.com/p-1062235395.html[21] Ministry of Agriculture. No. 1025-11 Bulletin of the Ministry of Agriculture of the People's Republic of China. (2008-04-29)[2015-02-10]. http://www.docin.com/p-1062235395.html 农业部.中华人民共和国农业部公告第1025-11号. (2008-04-29)[2015-02-10]. http://www.docin.com/p-1062235395.html

扫一扫看文章

计量

PDF下载量: 6
文章访问数: 426
HTML全文浏览量: 26

通讯作者: 陈斌, bchen63@163.com

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-超高效液相色谱-串联质谱法快速测定猪尿中15种β₂-受体激动剂残留

通讯作者: 曲宝涵,赵思俊; 曲宝涵,赵思俊

English

Rapid determination of 15 β ₂-agonists residues in swine urine by ultra performance liquid chromatography-tandem mass spectrometry coupled with molecularly imprinted solid phase extraction

Corresponding author: 曲宝涵,赵思俊; 曲宝涵,赵思俊

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

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

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？

计量

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-超高效液相色谱-串联质谱法快速测定猪尿中15种β2-受体激动剂残留

通讯作者: 曲宝涵,赵思俊; 曲宝涵,赵思俊

English

Rapid determination of 15 β 2-agonists residues in swine urine by ultra performance liquid chromatography-tandem mass spectrometry coupled with molecularly imprinted solid phase extraction

Corresponding author: 曲宝涵,赵思俊; 曲宝涵,赵思俊

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

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

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？

计量

文章相关

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-超高效液相色谱-串联质谱法快速测定猪尿中15种β₂-受体激动剂残留

Rapid determination of 15 β ₂-agonists residues in swine urine by ultra performance liquid chromatography-tandem mass spectrometry coupled with molecularly imprinted solid phase extraction

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs