Page 20 - Application Notebook - Solution for Food Safety
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Application  No.C136
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            Repeatability                                      Compounds were selected throughout the run at equi-
            To assess the robustness of the system and the     distant points (closest elution points to 3, 4, 5, 6, 7, 8,
            developed method during routine analysis, repeat   9 and 10 minutes), including positive and negative ion
            injections of a mint matrix sample spiked with 646   detection, (Table 3).
            pesticides at 0.05 mg/kg, were analyzed over a 24 hour   The peak area variance was less than 5.7 % for all
            period.                                            pesticides measured.
            The results for selected compounds are displayed below
            in Fig. 5.


             Peak Area Response
              Quantitation Ion
                     ×10 6
                 4.5

                 4.0

                 3.5


                 3.0


                 2.5

                 2.0


                 1.5


                 1.0

                 0.5


                 0.0
                    0       10       20      30       40      50       60      70       80      90      100
                                                       Number of injections
                     Butocarboxim-sulfoxide   Thiofanox-sulfone      Monolinuron             Probenazole
                     Dipropetryn             Pyraflufen-ethyl        Emamectin B1a           Pyridalyl

                Fig. 5  Peak area response for several pesticides following 100 repeat injections of a 0.05 mg/kg spiked into mint matrix extract.

                 Table 3  Peak area variance for selected following the repeated injection of a 0.05 mg/kg spiked into mint matrix extract
                       (number of sample replicates was 100; the analysis sequence was 24 hours).
                                                                             MRM
                                   CAS                                                 RT    Average   %RSD
               Compound Name                   Formula       M    Polarity Quantitation
                                  Number                                             (mins)   Peak Area  (n=100)
                                                                             Ion
             Butocarboxim-sulfoxide  34681-24-8  C7H14N2O3S  206.0725  +  207.10 >  75.10  3.042  1,220,391  2.6
             Thiofanox-sulfone  39184-59-3  C9H18N2O4S     250.0987  +   268.10 >  57.00  4.001  442,724  5.7
             Monolinuron        1746-81-2  C9H11ClN2O2     214.0509  +   215.10 >  99.10  4.985  2,904,116  3.7
             Probenazole        27605-76-1  C10H9NO3S      223.0303  +   224.00 >  41.05  5.995  1,145,189  3.5
             Dipropetryn        4147-51-7  C11H21N5S       255.1518  +   256.20 > 144.05  6.999  3,289,597  3.4
             Pyraflufen-ethyl   129630-19-9  C15H13Cl2F3N2O4  412.0204  +  413.00 > 339.00  8.004  3,653,333  3.5
             Emamectin B1a      138511-97-4   C56H81NO15  1007.5606  +   886.40 > 158.20  9.008  3,109,562  4.5
             Pyridalyl          179101-81-6  C18H14Cl4F3NO3  488.9680  -  491.90 > 109.05  10.171  1,579,422  5.0
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