超高效液相串聯(lián)質(zhì)譜法分析豬肉中殘留的15種β—受體激動(dòng)劑

歐貝麗++倪偉華++鄒+燕++趙佳麗

摘要 [目的]應(yīng)用超高效液相色譜串聯(lián)質(zhì)譜技術(shù)建立同時(shí)測(cè)定豬肉中15種β-受體激動(dòng)劑的檢測(cè)方法。[方法]樣品經(jīng)β-鹽酸葡萄糖醛苷酶/芳基硫酸酯酶酶解、0.2mol/L乙酸銨溶液（乙酸調(diào)pH至5.0）提取，陽離子固相萃取柱凈化，以0.01mol/L乙酸銨（含0.1%甲酸）-甲醇為流動(dòng)相梯度洗脫，C18柱為色譜柱進(jìn)行分離，串聯(lián)質(zhì)譜多反應(yīng)檢測(cè)（MRM）模式測(cè)定。[結(jié)果]15種β-受體激動(dòng)劑在5～100 ng/mL 濃度范圍內(nèi)線性關(guān)系良好，3種添加水平下樣品平均回收率在74.2%～115.6%之間。[結(jié)論]該方法提取效率高，凈化效果好，具有良好的靈敏度和準(zhǔn)確性，適合大批量豬肉樣品中15種β-受體激動(dòng)劑的快速測(cè)定。

關(guān)鍵詞 超高效液相色譜-串聯(lián)質(zhì)譜；豬肉；β-受體激動(dòng)劑；固相萃取

中圖分類號(hào) TS251.5+1 文獻(xiàn)標(biāo)識(shí)碼 A 文章編號(hào) 1007-5739（2015）12-0276-03

Determination of 15 β-agonists Residues in Pork by Ultra-performance Liquid Chromatography-mass Spectrometry

OU Bei-li NI Wei-hua ZOU Yan ZHAO Jia-li

（Jiaxing Institute for Food and Drug Control in Zhejiang Province，Jiaxing Zhejiang 314000）

Abstract [Objective]To develop a method for determination of 15β-agonists residues in pork by ultra-performance liquid chromatography-mass spectrometry.[Method]The samples were enzyme hydrolyzed by β-Glucuronidase/aryl sulfatase，etracted with 0.2 mol/L Acetic acid-ammonium acetate buffering solution（pH=5.0），and cleaned up on a SPE cartridge，separated on a C18 column using 0.01mol/L ammonium acetate（contain 0.1% Formic Acid）- Methanol as mobile phase，and detected under multiple reaction monitoring（MRM）mode.[Results]The resultes displayed a good linearity for 15β-agonists over the range of 5～100 ng/mL.The mean recoveries were from 74.2% to 115.6% at three different concentrations.[Conclusion]The method was precise，sensitive，and highly efficient in extraction and purification，and it is suitable for fast analysis of β-agonists residues in a large number of pork samples.

Key words ultra-performance liquid chromatography-mass spectrometry；pork；β-agonists；solid phase extraction

β-受體激動(dòng)劑，俗稱“瘦肉精”，是一類化學(xué)合成的結(jié)構(gòu)和功能類似于腎上腺素和去甲腎上腺素的苯乙醇胺類衍生物，用于治療支氣管哮喘、平滑肌痙攣等疾病[1]。人們?cè)谘芯窟^程中發(fā)現(xiàn)，其具有促進(jìn)肌肉組織生長、減少脂肪沉積的作用，一些養(yǎng)殖戶為追求更大經(jīng)濟(jì)效益在飼料中添加β-受體激動(dòng)劑，以改善豬肉品質(zhì)。但是由于這類藥物在飼料中的添加劑量較大，易在肉中殘留，人一次攝入一定量的高殘留的豬肉即可出現(xiàn)β-受體激動(dòng)劑的毒副作用[2]，近年來食用β-受體激動(dòng)劑殘留超標(biāo)的肉類導(dǎo)致的中毒事件時(shí)有發(fā)生[3]。因此，該類食品安全問題已越來越受政府部門的重視，針對(duì)β-受體激動(dòng)劑殘留的初篩和確證方法研究已成為近年來獸藥殘留研究的熱點(diǎn)[4-5]。……