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Gas Chromatography Mass Spectrometry Determination of Clenbuterol in Human Plasma

Lake, washed once with 4ml ethanol, centrifuged,[link widoczny dla zalogowanych], then washed again. Combined three supernatant 60m1 separating funnel, with 2mol · INaOH solution pH adjusted to 1O ~ 11, with chloroform 15,10, lOml extracted three times, combined extract, 3g of anhydrous sodium sulfate by dehydration, in the pan 5O ~ 6O ℃ in water bath, concentrated almost dry, add 2 drops of hydrochloric acid 2mol · L evaporated to dryness, residue dissolved with ethanol, transferred to 2ml volatile liquid storage bottle to dry, add ethanol 100/21 dissolved sample by GC-MS conditions analysis,[link widoczny dla zalogowanych], sample size 1_Ol. 2 Results and discussion 2.1 Determination of optimal conditions for GC-MS, according to the characteristics of clenbuterol, by changing the column temperature, heating rate, inlet temperature, GC-MS interface temperature and other conditions to scan each sample was observed The retention time of clenbuterol and the total ion current peak shape, to ensure good separation of the premise to shorten the retention time to determine the optimum chromatographic conditions; by selecting the major ion m/z86,[link widoczny dla zalogowanych], 57,127,41, 190,87 to observe the ion peak shape, see the matrix interference, and determine the 86 (base peak) for the quantitative ions, without interference 127,190,87 for qualified ions. 2.2 clenbuterol standard curve with a detection limit of the stock solution of clenbuterol was diluted with absolute ethanol 0. Ol, 0.05,0.1,0.5,1.0,2.5,10,50,100,200,400 ~ g · ml of standard liquid chromatography conditions for the SIM mode by injection determination of each about twice 1_Ol, integrated peak area. Clenbuterol in the range of 0.1 ~ lOOng linear regression equation is Y a 1.3O × 1OX a 654, r A 0.9999 (I 6), the detection limit was 0.05ng (N = 3). 2.3 The precision of the 1. Og · ml of standard solution of clenbuterol by GC-MS conditions for 6 parallel determinations, relative standard deviation was 2.859 / 6, good precision. 2.4 The test method is by the recovery test, take 13 centrifuge tube number 1 as the blank, the tube plus normal blood lml, 2 ~ 7 号 tube plus clenbuterol lO / ~ g, is determined 9.93/xg, recovery was 99.3, RSD is 3.879 / 6.8 ~ 13 tube plus clenbuterol 1g, measured value 0.956/xg, recovery was 95.6, RSD = 6.82. Blank without interference. Test found that adding clenbuterol lOng, if extracted with chloroform, concentrated by dehydration after constant volume direct injection, recovery was 98.1 (a 6, RSD = 6.09); if the chloroform extract and converted into clenbuterol hydrochloride, the recovery rate was 99.3, showing that the injection form of clenbuterol, and in the form of clenbuterol hydrochloride injection, consistent with the results. Chloroform extraction of biological samples, should prevent the formation of the emulsion layer. Test showed that the emulsion layer extraction process, there are more, the recovery will be reduced to 8O9 / 6. Available at this time or add a small amount of anhydrous sodium sulfate centrifugal method of removing the emulsion layer. 2.5 Determination of taking samples of patients with gastric poisoning each 2ml, 2mol · LNaOH solution with pH = 11,[link widoczny dla zalogowanych], extracted with chloroform, after dehydration, concentration, according to chromatographic conditions to scan sample analysis, the results were detected at 7.72min Clenbuterol. Then take the blood of the poisoned patients 5ml, according to test method extraction, the GC_MSIM analysis of the results measured in the blood of patients Clenbuterol contents were 0.018 and 0.026/xg · ml_. . Clenbuterol in biological materials derived directly without (MS method validation and quantification of the peak shape is good and stable, by selected ion monitoring (SIM3 remove large interfering ions 57,41 and other debris, eliminating the matrix effect. And MS compared to derivatization, eliminating the over solid phase column, derivatization and other steps, simple time-saving, and the method reproducible, high recovery rate is fast and accurate testing of biological material (such as patients with body fluids, animal tissue) effective method of Clenbuterol, it is appropriate to promote the use.
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