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High Performance Liquid Chromatography pork Clenbuterol

0), oscillating extraction 20min. Extraction is completed, place 5min (if slightly eccentric about the emulsion layer.) Carefully with a straw to move the upper layer of the organic phase rotary evaporator flask, with 2Oml isopropyl alcohol + ethyl acetate (40 +60) and then repeat the extraction time, combined organic phase, evaporation at 6O ℃ to nearly dry. (With 1.00ml of sodium dihydrogen phosphate buffer (O.010mol/1pH6.O) fully dissolve residue) after filtration and set the volume fully transferred to 5ml (or fully dissolve residue 0.50ml ethanol, centrifuged, the supernatant reserve liquid). Solution was 0.45m above the sample processing membrane filtration reserve, and the injection 1Ol. 2.2 Determination of standard solution 0.00,2.00,4.00,[link widoczny dla zalogowanych],6.00,8.00,10.00,2 O. lessons 00gg/ml and sample, sample 1O. 001 analysis, with the retention time qualitative and quantitative peak area. 2.3 Calculation of X a {(m/1000) / 1000) / {(M/1000) / vI) × (V2/1000) where, X: concentration of clenbuterol hydrochloride in samples (mg / kg); M: sample sample volume (g); m: samples of clenbuterol (ng); V: sample volume at constant volume (m1); V; sample injection volume (1). 3 Results and discussion 3.1 acetonitrile mobile phase using a choice of O. 010mol / L of KHzPO (pH a 3.50) system, a H0 methanol system, the separation of clenbuterol are not ideal (mainly the interference of impurities in the sample.) However,[link widoczny dla zalogowanych], a methanol O. 010613mol / L of KH2PO (pH = 3.50) system, the separation effect. A methanol O. 010mol/LKH2PO (pH = 3.50) in 5 / 95 ~ 5o/5o experiment with different ratios, the best separation for the 33/67. 3.2 the choice of column temperature increased the column temperature is conducive to lower mobile phase viscosity , improve column efficiency, help speed up the peak time, in the 20 to 45. Choose between C to 35 ℃ best, the analysis time is only about 6.5min. 3.3 Wavelength clenbuterol in 211nm,[link widoczny dla zalogowanych], 243nm, 298nm3 an absorption wavelength are absorbed, but the absorption peak decreased gradually, considering the sensitivity, linear range and spectral interference and other factors, the detection wavelength was 243nm selected . Linear relationship and the detection limit of 3.4 standard solution 0.00,2.00,4.00,6.00,8.00,1 O. lessons 00,[link widoczny dla zalogowanych],2 O. 00 ~ g / ml; standard curve (A 7), the linear range of O ~ 20.00gg/ml, the mean peak area were: 79126,148735,231786,318685,380012,776847 regression equation X: 2. 57957 × 10y +0, the correlation coefficient r = 0. R994. The detection limit (by instrument noise, in response to 3 times the value of sample size calculation) 0.56 ~ g / kg. 3.4 3.4.1 The accuracy and precision experiments within the linear range precision of high, medium and low 3 clenbuterol standard solution and determination of sample repeat 5 times, the results of standard solution of clenbuterol The relative standard deviation (rsd) 6.35% ~ 8.36%, the sample relative standard deviation (rsd) 10.58% ~ 11.36%. 3.4.2 copies of accuracy in 6 different samples were added to 2O, 8O, 100ng recovery of clenbuterol determined standards, the end of 3 parallel with the recovery experiments were measured 5 times, the results of the recovery 8O. 54 ~ 89.32, and the relative standard deviation (rsd) 11.23 ~ 12.36. 3.5 interference interference experiment samples mainly from the processing and purification, handle it properly without obvious interference. 3.6 Qualitative clenbuterol mouth] rely mainly on GC / Ms, HPLC / MS characterization; in the absence of GC / Ms,[link widoczny dla zalogowanych], HPLC / Ms under the conditions of HPLC peaks can use cutting-edge, the peak point, the peak along the 3-point Determination of peak purity, the purity factor calculated for qualitative, but also to retrieve the standard atlas. [
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