液相色譜-串聯(lián)質(zhì)譜法測定育肥豬配合飼料中的阿奇霉素
發(fā)布時間:2018-06-03 17:12
本文選題:液相色譜-串聯(lián)質(zhì)譜(LC-MS/MS) + 阿奇霉素 ; 參考:《分析測試學報》2017年03期
【摘要】:通過對提取溶劑、凈化方法及色譜-質(zhì)譜條件的優(yōu)化,建立了配合飼料中阿奇霉素(AZM)的液相色譜-串聯(lián)質(zhì)譜測定方法。樣品經(jīng)乙腈超聲波提取,MCX固相萃取柱凈化,BDS Hypersil C_(18)(2.4μm,100 mm×2.1 mm)色譜柱分離,以甲醇-0.05 mol/L乙酸銨水溶液為流動相梯度洗脫,正離子模式電離,多反應(yīng)監(jiān)測模式檢測,同位素內(nèi)標法定量。在優(yōu)化條件下,AZM在1~250μg/L范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)(r~2)為0.999 1,檢出限(S/N≥3)為2.8μg/kg,定量下限(S/N≥10)為8.4μg/kg;在0.5,1,5,10 mg/kg加標水平下,回收率為87.0%~106.6%,批內(nèi)相對標準偏差為0.58%~5.4%,批間相對標準偏差為3.1%~5.4%。該方法準確、靈敏,選擇性強,基質(zhì)干擾小,可用于配合飼料中AZM的測定。
[Abstract]:A liquid chromatography-tandem mass spectrometry (LC-MS) method for the determination of azithromycin (AZM) in compound feed was established by optimizing the extraction solvent, purification method and chromatography-mass spectrometry conditions. The samples were purified by ultrasonic extraction with acetonitrile and purified on the column of BDS Hypersil (182.4 渭 m). The mobile phase gradient elution was methanol-0.05 mol/L ammonium acetate solution, the positive ion mode ionization, the multi-reaction monitoring mode detection and the isotope internal standard method. Under the optimized conditions, the linear range of AZM is 1: 250 渭 g / L, the correlation coefficient is 0.999 1, the detection limit S / N 鈮,
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