Gemcitabine Gemzar spectrometer with an electrospray interface under the following

Min, linear ramp to 260 ° C at 4 ° C min -1 and held for 1 min, and further increased to 280 C at 10 ° C min1 Ht. The MSD was Gemcitabine Gemzar operated in electron ionization mode at 70 eV. Liquid chromatography / hybrid quadrupole time of flight mass spectrometry for the identification of polar by-products used. The chromatographic conditions are the same as above in the determination of alachlor by HPLC. Operated with an HPLC-TOF mass spectrometer with an electrospray interface under the following conditions attached: 3.50 kV capillary voltage 20 V c has, source temperature 120 ° C, desolvation temperature of 300 ° C and collision energy of 5 eV. Accurate mass measurements were recorded at a resolution and high of more than 5,000 independently with the help of a Ngigen reference spray via St Ensure the accuracy requirements LockSpray performed. Propachlor was used as internal lock mass m / z 212.0842. All data were processed using MassLynx version 4.0, MS. 2 3 Hydro chloroacetyl indole acetyl ketone 7th It has a parent ion at m / z 251 of the 37Cl at m / z 253rd The m / z 253 ion in CH 2 Cl lose k The chloroacetyl group nnten to m / z 202 to give, and YOUR BIDDING lose the chloroacetyl group at m / z 174 to give. This compound has not been reported so far. Compound 13 with RT 36.5 min and 297 MW, k Nnte 2 N 20.60 chloro acetanilide diacetyl. It has a parent ion at m / z 297 with the 37Cl corresponding to m / z 299th Similar to the fragmentation of alachlor molecular ion, the molecular ion of compound 13-297 M lose z / CH 3 OH in the methoxymethyl group k Nnte to give m / z 265, and YOUR BIDDING lose the game methoxymethyl m / give z 252nd This compound has not been reported so far. Compound 14 with RT 37.2 min and 283 MW, k Nnte 2 20 60 acetyl chloride Ethyl-N may be acetanilide. The molecular ion at m / z 283 ion with a chlorine isotope at m / z 285 k losing yield Nnte Cl m / z 248th The spectrum is consistent with the previously reported. This compound was detected as a degradation product of alachlor in groundwater. For the HMW relatively polar by-products which were difficult to detect by GC / MS, LC was generally the preferred. The efficacy of the combination of LC / Q-TOF-MS / MS and GC / MS techniques in the identification of unknown by-products detected. The LC / Q-TOF-MS / MS chromatograms showed that sold both direct ozonation and by-products of degradation O3/H2O2 several alachlor. Table 1 shows the measured and calculated masses of ions by-products, the error between them and the proposed empirical formula of the compounds identified by LC / Q-TOF-MS / MS. Zus Best tzlich to information from the protonated molecular ion, the presence of sodium adducts Preferential the identity t analytes, so the information is accurate mass fragments characteristic facilitates the assignment of structure. It should be noted that all protonated molecular ions or sodium adducts corresponding own 37Cl isotopes battery had to best Confirmation displayed. Based on the exact mass of the protonated molecular ion of compound I has the formula has been proposed, with a low error rate C12H13NO3Cl. The style of fragmentation was Similar to the by GC / MS for compound 8, was therefore referred to as 2-chloro acetyl acetanilide 20,60. The formation of the ketone group, double bond Equivalence, which represents the number of rings and pads.

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