. 3.4. Optimization of the mobile phase for RRLC MS / MS Agilent Optimizer software was used to JNJ 26854165 Serdemetan optimize operating conditions LC MS / MS ionization modes for both positive and negative by infusion of standard L Solutions. The base peak for the quantification of estrogen study selected hlt Corresponds to the deprotonated molecule Androgens, progestins and glucocorticoids Of were detected with the protonated molecules. The instrumental conditions in the negative mode Estrogens have been optimized in our previous study, with pure water and acetonitrile as mobile phase. Solvents to the operating conditions in the positive mode, two organic And optimize different phases of water were tested. The best operating conditions were obtained with w Formic ssriger Acid.
Although a better peak shape with acetonitrile as the organic L Solvents were obtained, methanol was used in this study to a better separation for all analytes 24 with To obtain similar structures. Thus the optimized mobile phases: Acetonitrile and pure water for the analysis of strogenen in the negative mode, and methanol and 0.01% formic acid-L solution for the analysis of androgens, progestins, and glucocorticoid in the positive mode. 3.5. Effect matrix matrix effect is acommonproblem for LC-MS / MS with ESImode that lead to the elimination or improvement of the signal can k, And is often difficult to remove by cleaning procedures. Matrix effects were observed and Zus Conversions of standard L Solutions in the extract samples from surface Chenwasser, wastewater and plaintiff examined rschlamm.
Values of less than or more than 100% denotes signal suppression or reinforcing Rkung respectively. The results in Tables 4 6 showed that matrix components in the surface Chenwasser or wastewater had no significant effect on the response signals of the target compounds for internal standard correction had. But matrix components in the samples of feed response signal 17 trenbolone, trenbolone 17, ADR, DES, returned with matrix effects from 41.9 to 68.0% but increased signal responses prednisone, dexamethasone and MP, with matrix included 132 of 186%. Matrix components in the sludge samples were also reduced signal responses of cortisone, prednisolone, ADR, and EE2. 3.6. Calibration curves of the validation method was to androgens from 1.0 to 1000 g / l and built for other targets from 1.
0 to 200 g / l and an excellent linearity of t obtained in this concentration range with correlation coefficients gr It as 0.99 for all the validation batches. With the optimized extraction and instrumental analysis, good recoveries for all target compounds in the matrix samples were water samples, wastewater and sludge surface Will surface. The detection limit and quantitation limit for each target compound was based on the signal to noise ratio Ratio in the N He calculates the target peak flow. LOD is defined as three times the SNR, and LQ is ten times more SNR. The quantification limits for the target analyte in the feed, waste water surface Chenwasser, and freeze-dried sludge samples were 0.05 4.8 0.02 1.63 0.03 0.80 ng / L, 0.3 and 6.9 ng / g on. This dose ranges of compounds in hours Higher inflows and freeze-dried samples sludge in the sewage and surface water were Chenwasser probablyTwosurface, tw Lf and eight plaintiff were rschlamm samples were analyzed in comparison of the advanced countries
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