饲料中抗生素检测方案(固相萃取仪)

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Application Note 903FOOD AND BEVERAGERT-AP-903 自动固相萃取仪用于动物饲料中的抗生素(抗菌素)检测 介绍： 饲料如玉米，谷物，大米等样品正常需要检测抗生素类，此方法用于从家禽饲料中提取和净化泰妙菌素(Tiamulin hydrogen fumarate)，同时也可用于同类抗生素的化学分析. 样品预处理 取25克样品饲料加入氯仿150毫升和碳酸钠10毫升混合液，摇晃30分钟，再加入100毫升乙腈，短暂摇晃后滤出10毫升样品到16mm*100mm样品管中等待 rt 自动固相萃取.自动固相萃取仪采用1毫升填有130毫克的 scx 填料的萃取小柱，用1毫升的洗脱液a(乙酸铵：乙腈， ph10)洗脱后，收集样品用1毫升溶液b中和(乙酸铵：乙腈， ph1)，取1毫升样品转移到2毫升样品管中，20微升的样品被注入 HPLC 分析. RT方法编辑 步骤 溶剂/来源 排出口 体积(毫升) 流量(毫升/分钟) 活化 condition ACETONITRILE 乙腈 有机废液口Organic waste 3 15 加样 load 样品 Sample 有机废液口 Organic waste 5 2 加样 load 样品 Sample 有机废液口 Organic waste 5 2 淋洗 rinse 甲醇Methanol 有机废液口Organic waste 2 5 淋洗 rinse ACETONITRILE 乙腈 有机废液口 Organic waste 2 5 吹干dry 氮气Nitrogen 4分钟4minute 20Psi 清 洗 purgecannula ELUENTa洗脱液a(乙酸铵：乙，ph10) Cannula watste 2 0.5 收集 collect ELUENTa洗脱液a(乙酸铵：乙腈，ph10) 收集管1Fraction1 1 30 清 洗 purgecannula WATER水 Cannula watste 2 2 清 洗 purgecannula 甲醇Methanol Cannula watste 2 2 清 洗 purgecannula ACETONITRILE乙腈 Cannula watste 2 2 Automated Solid Phase Extraction forAntibiotics in Animal Feed Introduction It is common practice to incorporate antibiotics in animal feedstuffs such as corn， rice andmaize. This method describes how to extract and cleanup a sample of Tiamulin HydrogenFumarate from poultry grain although it is possible this method will work for a range ofantibiotics. Instrumentation Used for Sample Preparation TurboVap LV for Automated Sample Evaporation Sample Preparation A 25g sample of feedstuff is shaken for 30 minutes with Chloroform (150mL) and So-dium Carbonate (10mL) mixture to extract the antibiotic. Acetonitrile (100mL) is thenadded and after a brief shake a 10mL sample is filtered into a 16mm x100mm vial readyto be cleaned up automatically by the RapidTrace. The Solid Phase Extraction is carriedout using a 1mL Isolute cartridge filled with 130mg of SCX packing material. Followingextraction the 1mL of eluent A (Ammonium Acetate： Acetonitrile， pH10) is neutralisedwith 1mL of eluent B (Ammonium Acetate： Acetonitrile pH1). A 1mL sample is trans-ferred to a 2mL vial and 20uL is injected onto the HPLC for analysis. RapidTrace Overview The RapidTrace is an automated Solid Phase Extraction instrument capable of preparing10 samples. It has a modular design so multiple RapidTrace units can increase thethroughput without risk of downtime due to the independence of each instrument. All solvent lines are purged and primed with solvent first. A maximum of 8 solvents can be used torun a wide range of methods. The 4 independent waste solvent lines can be separated if needed.The instrument sample rack has two rows of 10 test tubes， 16mm x100mm for holding the sam-ples and eluent fractions. This method offers an automated，rugged and reproducible solution forcleaning up the samples to remove interferences. The RapidTrace Method SOURCE DESTINATION VOLUME FLOW (ML/MIN) Condition Acetonitrile Organic Waste 3.0 15.0 Sample Organic Waste 5.0 2.0 Load Sample Organic Waste Methanol Organic Waste Acetonitrile Organic Waste 2.0 Nitrogen Gas 4 minutes (20 psi) Purge Cannula EluentA Cannula Waste 30.0 EluentA Fraction 1 0.5 Purge Cannula Water Cannula Waste 2.0 30.0 Purge Cannula Methanol Cannula Waste 2.0 30.0 Purge Cannula Acetonitrile Cannula Waste 2.0 30.0 Common Reagent Table for All Methods CaliperLifeSciences Corporate Headquarters68 Elm StreetHopkinton， MA01748-1668 Tel： 508 4369500Fax： 508 435 3439 C2008 Caliper Life Sciences. All rights reserved.Caliper，， theCaliperr logo， AutoTrace，RapidTrace， and TurboVap are trademarks orregistered trademarks of Caliper Life Sciences.All other trademarks contained herein are theproperties of their respective owners. Email： cust.support@caliperLS.com www.caliperLS.com