凝胶净化色谱-固相萃取-超快速液相色谱-串联质谱法检测猪肉中9种β2-受体激动剂激素残留

doi:10.7506/spkx1002-6630-201224068

食品科学 ›› 2012, Vol. 33 ›› Issue (24): 311-314.doi: 10.7506/spkx1002-6630-201224068

凝胶净化色谱-固相萃取-超快速液相色谱-串联质谱法检测猪肉中9种β2-受体激动剂激素残留

卢剑1，车文军1，张岩2,*，庞坤2，李挥2，武中平1

1.江苏省产品质量监督检验研究院，江苏南京 210007；2.河北省食品质量监督检验研究院，河北石家庄 050091

收稿日期:2012-05-22 修回日期:2012-11-12 出版日期:2012-12-25 发布日期:2012-12-12
通讯作者: 张岩 E-mail:snowinglv@126.com

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

LU Jian1，CHE Wen-jun1，ZHANG Yan2,*，PANG Kun2，LI Hui2，WU Zhong-ping1

1. Jiangsu Province Products Testing and Inspection Institute, Nanjing 210007, China；2. Hebei Institute of Food Quality Supervision Inspection and Research, Shijiazhuang 050091, China

Received:2012-05-22 Revised:2012-11-12 Online:2012-12-25 Published:2012-12-12

摘要/Abstract

摘要： 建立凝胶净化色谱-固相萃取-超快速液相色谱-串联质谱(GPC-SPE-RRLC-MS/MS)测定猪肉中β2-受体激动剂激素残留(沙丁胺醇、西马特罗、特布他林、克伦特罗、莱克多巴胺、氯丙那林、喷布特罗、妥布特罗、非诺特罗)的方法。试样经β-盐酸葡萄糖醛苷酶/芳基硫酸酯酶酶解，叔丁基甲醚超声提取，凝胶净化色谱和HLB柱净化，以甲醇-0.1%甲酸溶液为流动相，经Agilent Plus C18柱分离后进行RRLC-MS/MS多反应监测扫描模式分析检测。方法线性相关系数r＞0.996，检出限为0.1～0.3μg/kg，在0.3、2.0、5.0μg/kg 3种添加水平的平均回收率为79.35%～109.80%；相对标准偏差为2.12%～9.11%。该方法灵敏度高、重现性好、定性定量准确，适用猪肉样品检测。

关键词: 超快速液相色谱-串联质谱, β2-受体激动剂激素, 凝胶净化色谱, 固相萃取, 猪肉

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

中图分类号:

O657.6

卢剑1，车文军1，张岩2,*，庞坤2，李挥2，武中平1. 凝胶净化色谱-固相萃取-超快速液相色谱-串联质谱法检测猪肉中9种β2-受体激动剂激素残留[J]. 食品科学, 2012, 33(24): 311-314.

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凝胶净化色谱-固相萃取-超快速液相色谱-串联质谱法检测猪肉中9种β2-受体激动剂激素残留

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

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