【摘要】：建立了分散固相萃取-同位素稀釋-高效液相色譜-串聯(lián)質(zhì)譜(dSPE-ID-HPLC-MS/MS)同時(shí)測定豬肉中26種β-受體激動(dòng)劑殘留的方法。樣品經(jīng)β-葡萄糖醛苷酶/芳基硫酸酯酶水解12 h后,用高氯酸沉淀蛋白質(zhì),取上清液,調(diào)節(jié)pH值為9,用乙腈渦旋提取,分散固相萃取凈化。選用具有混合分離模式的新型色譜柱Poroshell 120Phenyl-Hexyl(100 mm×2.1 mm,4.0μm)對(duì)待測物進(jìn)行分離,在電噴霧離子(ESI)源正離子模式下以多反應(yīng)監(jiān)測(MRM)模式采集數(shù)據(jù)并做定性篩查和定量分析。26種待測物在相應(yīng)的濃度范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)均大于0.99,在3個(gè)不同濃度的添加水平下,平均回收率為65.3%~108.5%,相對(duì)標(biāo)準(zhǔn)偏差(RSD)為2.7%~13.3%,檢出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分別為0.03~0.1μg/kg及0.1~1.0μg/kg。該方法成本低廉、靈敏可靠,適用于同時(shí)對(duì)豬肉產(chǎn)品中26種β-受體激動(dòng)劑殘留進(jìn)行定性和定量篩查。
[Abstract]:A method for simultaneous determination of 26 尾 -agonist residues in pork by dispersive solid-phase extraction, isotope dilution, high performance liquid chromatography-tandem mass spectrometry (dSPE-ID-HPLC-MS/MS) was developed. The sample was hydrolyzed by 尾 -glucuronidase / aryl sulfate for 12 h, then the protein was precipitated with perchloric acid, the supernatant was extracted, the pH value was adjusted to 9, extracted by acetonitrile vortex, and purified by dispersive solid-phase extraction. A new Poroshell 120Phenyl-Hexyl (100 mm 脳 2. 1 mm,4.0 渭 m) column with mixed separation mode was used to separate the determination. In the positive ion mode of electrospray ion (ESI) source, the data were collected by multi-reaction monitoring (MRM) mode, and the qualitative screening and quantitative analysis were done. The linear relationship of 26 kinds of samples was good in the corresponding concentration range, and the correlation coefficients were all greater than 0.99. At three different concentration levels, the average recovery rate was 65.3% and 108.5%, and the relative standard deviation (RSD) was 2.7and 13.3.The detection limit (LOD,S/N=3) and the quantitative limit (LOQ,) were obtained. The S/N=10 was 0.03 渭 g/kg and 0.1 渭 g / kg, respectively. The method has the advantages of low cost, high sensitivity and reliability. It is suitable for qualitative and quantitative screening of 26 尾-agonist residues in pork products at the same time.
【作者單位】： 中國廣州分析測試中心廣東省分析測試技術(shù)公共實(shí)驗(yàn)室;
【基金】：廣東省科技計(jì)劃項(xiàng)目(2014B070705001) 廣州市科技計(jì)劃項(xiàng)目(11BppZXcc6100034)~~
【分類號(hào)】：O657.63;TS251.7

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