| The abuse and illegal usage of veterinary medicine does great harm to national even global environment and human body health. Steroid hormone is a kind of lipophilic and hydrophobic compound and it belongs to the category of veterinary medicine. It is usually and widely used in livestock breeding as protein anabolic agen.The long-term abuse of this veterinary medicine increases the risk of carcinogenic and teratogenicity, meanwhile, it caused people’s high attention about the analyzing of its residues. So,there is important significance in researching the detection and analysis methods of the residual state of steroid anabolic hormone in products of animal origin.This paper studies steroid hormones including Trenbolone, Boldenone,Testosteron,17-alpha-methyltestosterone,19-Nortestosterone,Metandienone,Progesterone,Dexamethasone,6-alpha-Methylprednisolone, Meprednisone,Triamcinolone,Triamcinolone Acetonide.The sample matrix: chicken and beef.It adopted ultra performance liquid chromatography-tandem mass spectrometry to detect and analyze the residues.Two methods to detect the residues of steroid anabolic hormone in products of animal origin have been comparatively studied in this paper:traditional solid-phase extraction and matrix solidphase dispersion method.This paper studied the linear,recovery and reproducibility and test and verify the reliability of the methods. The main research results are as follows:(1) Establishmenu of analysis method Select MRM for signal acquisition of the standard mixture solution. Adopt the positive and negative ion mode, select the suited molecular ion peak and ionization of the target compound and scanned by the daughter ion at the same time to fix the characteristic ion.By optimizing the condition of liquid chromatogram to final fix to use chromatographic column ACQUITXUPLC HSS T3to separate the target compound.To use acid water by methanol5mmol and aceticacid0.1%as the mobil phase gradient to elution, the current velocity is0.4ml/min,the column temperature is40centigrade to detect.The12kinds of target compound could be completely separatedwithin6min.(2) Sample pre-treatment method comparison Solid phase extraction(SPE):the sample be extracted by the acetonitrile and be purified by the solid phase extraction column Oasis HLB and be eluted by methanol-acetonitrile mixtures and after be blew by nitrogen and be dissolved by the acetonitrile water. Matrix solid-phase dispersion(MSPD):Extracted by1%acetic acid,purified by the matrix solid phase pipe,nitrogen blow enrichment,deluted by acetonitrile water. On the foundation of solid phase extraction,simplified and shortened the pretreatment, provide the theory foundation for the short-term test.(3) Methodology validation The linearity of the standard curve of two method is well r>0.99,Solid phase extraction detected the LOD is between0.3and1.0μg/L. The average recovery in beef were detected as from percentage64.75to percentage112.53,relative standard deviation as between percentage4.63and percentage11.21.The average recovery in chicken were detected as from perce ntage72.48to percentage114.52,relative standard deviation as between percentage3.93and percentage11.17.The recovery and precision of this method both meet the demand of residual analyzing. Matrix solid-phase dispersion detected the LOD is between0.2and0.8μg/L. The average recovery in beef were detected as from percentage72.7to percentage116.56,relative standard deviation as between percentage1.66and percentage11.3. The average recovery in chicken were detected as from percentage76.16to percentage123.3,relative standard deviation as between percentage3.4and percentage11.78.The recovery and precision of this method both meet the demand of residual analyzing.The MSPD method detection limit lower, higher recovery and pre-treatment is relatively simple. |
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