HPLC Analysis Of Anabolic Hormones Residues In Animal Mouscle

This study by chromatography and mass spectrometry and sample processing conditions, the system optimization established 15 kinds of anabolic hormones(Estriol, 17-beta- Estradiol, Estrone, 17-alpha- Ethiny lestradiol, Testosterone, 17-alpha- Methyltestosterone, Testosterone 17-propionate,Trena-bolone,19-Nortestosterone,Progesterone,Medroxyprogesterone-17-aceta- te, Hexestrol, Clenbuterol-hydrochloride, Diethylstilbestrol, Ractopamine- hydrochloride) high performance liquid chromatography (HPLC) and liquid chromatographic separation- tandem mass spectrometry (LC-MS/MS) detection methods. The Limit of quantification (LOQ) and Limit of detection (LOD) of the method acquire the requirement of the actual residual monitoring.1) A comfirmative method was developed with HPLC to detect anabolic hormones. Diode array detector was used at 230nm wavelength test. HYPERSIL BDS column for separation column and column temperature for 25°c, mobile phase for acetonitrile: 4mmol/L sodium heptanesulfonate-5% acetonitrile (V/V) solution gradient system.With the LOD 3.097-19.876μg/ Kg, LOQ10.322-66.239μg/Kg,the method is sensitive and reliable.2)The conditions for the extraction,such as extraction solvent,lipid filtration methed and solid-phase extraction were optimized.The treatment involves extraction of the analytes with methanal, freezing-lipid filtration at 0℃and clean-up by SPE with a Bond Eult C18 (500 mg,3mL). The recovery of spiked pig samples is 66.1%-113.9% and the relative standard deviation (RSD) is 2.1-12.4%.3)A method with LC-MS/MS to dectect residues of fifteen anablic hormones in meat food was developed.Multi-reaction monitoring (MRM) scan type with tandem mass analyzer using positive polarity mode for the androgen and progestational hormones, negative polarity for the estrogen respectively. The recovery of spiked samples is 64.0%-112.7% , the RSD is 1.0-22.2%,the LOD is 0.2-1.6μg/ Kg and the LOQ is 0.7-5.1μg/Kg.Applied with the analytical method erected,the residues of anablic hormones in the marking samples and detected successfully and satisfying results were obtained.