Determination of Nine β2-Agonist Hormones Residues in Pork by GPC-SPE-RRLC-MS/MS

doi:10.7506/spkx1002-6630-201224068

Abstract

Abstract: A gel permeation chromatography-solid phase extraction-rapid resolution liquid chromatography-tandem mass spectrometry (GPC-SPE-RRLC-MS/MS) method for the determination of 9 β2-agonist hormones including salbutamol, terbutaline, cimeterol, fenoterol, clenbuterol, ractopamine, clorprenaline, tulobuterol and penbutolol in pork has been developed. Pork samples were hydrolyzed with β-glucuronidase/arylsulfatase, extracted with tert-butyl methyl ether under ultrasonic incubation and cleaned up using gel permeation chromatography followed by solid phase extraction on an HLB column. After RRLC gradient elution separation on an Agilent Plus C18 column using methanol-water containing 0.1% formic acid as a mobile phase, the pooled eluate was qualitatively and quantitatively determined by tandem mass spectrometry under multi-reaction monitoring (MRM) mode. The limits of detection of this method were 0.1–0.3 μg/kg, and the developed calibration curves revealed excellent linearity with correlation coefficients larger than 0.996. At spiked levels of 0.3, 2.0 μg/kg and 5.0 μg/kg, average recovery rates of 9 β2-agonist hormones were in the range of 79.35%–109.80%, with RSDs between 2.12% and 9.11%. This method was sensitive, reproducible, accurate and applicable for the determination of β2-agonist hormones in pork.

Key words: RRLC-MS/MS, β2-agonist hormones, gel permeation chromatography (GPC), solid phase extraction (SPE), pork

CLC Number:

O657.6

References

[1] 李俊锁, 邱月明, 王超. 兽药残留分析[M].上海:上海科技出版社, 2002.
[2] Yantu Zhang, Zhujun Zhang, Yonghua Sun, et al. Development of an Analytical Method for the Determination of β2-Agonist Residues in Animal Tissues by High-Performance Liquid Chromatography with On-line Electrogenerated [Cu(HIO6)2]5--Luminol Chemiluminescence Detection[J]. J. Agric. Food Chem., 2007, 55(13): 4949–4956.
[3] 朱坚,李波,方晓明,等.气相色谱/质谱法测定肝、肾和肉中11种β2受体激动剂残留量[J].质谱学报, 2005, 26(3): 129-137.
[4] Caban M, Stepnowski P, Kwiatkowski M, Determination of β-blockers and β-agonists using gas chromatography and gas chromatography-mass spectrometry--a comparative study of the derivatization step[J]. J Chromatogr A, 2011, 1218(44): 8110-22.
[5] Daniele Di Corcia, Veronica Morra, Marco Pazzi, et al. Simultaneous determination of β2-agonists in human urine by fast-gas chromatography/mass spectrometry: method validation and clinical application[J]. Biomedical Chromatography, 2010, 24(4): 358–366.
[6] COLLINS S, O’KEEFFE M, SMYTH M R. Multi-residue analysis for beta-agonists in urine and liver samples using mixed phase columns with determination by radioimmunoassay [J]. Analyst, 1994, 119(12): 2671-2674.
[7] HAASNOOT W, STOUTEN P, LOMMEN A. Determination of fenoterol and rectopamine in urine by enzyme immunoassay[J] . Analyst, 1994, 119(12): 2675-2680.
[8] 余建新,胡小钟. HPLC/MS测定动物组织及尿样中的β2兴奋剂[J].分析测试技术与仪器, 2004, 10(4) : 244-247.
[9] 金玉娥,郭德华,郑烨,等. 液质联用仪测定动物源性食品中11种β2受体激动剂的研究[J].质谱学报, 2007, 28(4) : 193-201.
[10] 白凌,陈大舟,李蕾,等. 液相色谱-质谱法检测肝脏中5种β2受体激动剂[J].质谱学报, 2008, 29 (1) : 11-17.
[11] 孙雷,张骊,朱永林,等. 超高效液相色谱-串联质谱法检测动物源性食品中残留的9种β2受体激动剂[J].质谱学报,2008, 26 (6): 709-713.
[12] 吴永宁,苗虹,范赛,等. 高效液相色谱-线性离子阱质谱法测定畜禽肌肉中β2-受体激动剂及β-阻断剂类药物残留[J].中国科学B辑:化学, 2011, 39 (8): 774-784.
[13] 聂建荣,朱铭立,连槿,等. 高效液相色谱-串联质谱法检测动物尿液中的15种β-受体激动剂[J].色谱, 2010, 8 (8): 759-764.
[14] YongNing Wu, Hong Miao, Sai Fan, et al. Determination of 23 β2-agonists and 5 β-blockers in animal muscle by high performance liquid chromatography-linear ion trap mass spectrometry[J]. SCIENCE CHINA Chemistry, 2010, 53(4): 832-840.
[15] Hing-Biu Lee, Kurtis Sarafin, Thomas E. Peart. Determination of β-blockers and β2-agonists in sewage by solid-phase extraction and liquid chromatography–tandem mass spectrometry[J]. Journal of Chromatography A, 2007, 1148(2): 158-167.