Page 22 - Application Notebook - Solution for Food Safety
P. 22

Application  No.C136
    News

            Reducing matrix effects by extensively diluting    Fig. 8 shows the results of diluting a matrix sample
            the sample                                         spiked at 0.005 mg/kg with dilution factors of 1:5,
            The need to test for more pesticides in a wider range of   1:10, 1:20, 1:50 and 1:100.
            samples at high sensitivity is very challenging as matrix   As matrix effects can be both significant and variable
            effects from the sample extraction will influence both   for different compounds Table 4 shows recovery data
            ion suppression and enhancement. Ion suppression can   for a series of pesticides diluted from 0 to a dilution
            lead to errors in the detection capability, accuracy and   factor of 1:100.
            precision of the method.                           Matrix suppression was reduced for most compounds
            To reduce the effect of interfering compounds in the   when the sample was diluted 1:10 with recoveries in
            quantitation of complex samples extensive sample   the range of 70 - 120 % with an associated
            dilution is now widely used in routine analysis. It is an   repeatability RSDr ≤ 20 %. Relative standard deviations
            approach which is simple to build into multi-residue   in relation to the mean values were typically less than
            extraction methods and is cost effective.          10 %.
            This approach leads to greater robustness as a     Diluting the sample by a factor of 20 or 50 resulted in
            consequence of a reduced sample injection in the LC/  acceptable signal suppression from the matrix.
            MS/MS, higher data quality and increased instrument
            uptime.




               Bentazone    1:0             1:5          1:10            1:20            1:50          1:100







               Dimethoate   1:0             1:5          1:10            1:20            1:50          1:100







               Diphenamid   1:0             1:5          1:10            1:20            1:50          1:100








                          Fig. 8  MRM chromatograms for 3 selected compounds spiked into a mint extract at 0.005 mg/kg
                               and diluted 1:5, 1:10, 1:20, 1:50 and 1:100 with water.

                      Table 4  Diluting a sample matrix extract spiked with 0.005 mg/kg with water reduced matrix ion suppression.
                                                                  Dilution series
                   Compound          CAS       Formula       M        0      1:5   1:10   1:20   1:50  1:100
                                                                  Recovery
             Bentazone            25057-89-0  C10H12N2O3S  240.0569    32.1   44.6   65.5   72.7   91.7  98.1
             Demeton-S-methyl-sulfone  17040-19-6  C6H15O5PS2  262.0099  51.1  78.5  89.6   91.1  114.2  116.8
             Dimethoate           60-51-5   C5H12NO3PS2    228.9996    36.2   65.3   88.5   92.2   92.4  94.2
             Isocarbamid          30979-48-7  C8H15N3O2    185.1164    28.8   57.1   81.8   98.7  102.5  96.4
             Vamidothion          2275-23-2  C8H18NO4PS2   287.0415    53.6   76.3   98.2   98.5  101.5  114.1
             Thiazafluron         25366-23-8  C6H7F3N4OS   240.0293    32.8   62.9   80.5   84.2   87.1  97.4
             Demeton-S-methyl     919-86-8  C6H15O3PS2     230.0200    57.8   82.1   93.1   87.6  108.5  102.4
             Sebuthylazine        7286-69-3  C9H16ClN5     229.1094    28.7   53.3   69.8   79.8   88.5  95.8
             Flutriafol           76674-21-0  C16H13F2N3O  301.1027    27.3   46.1   71.4   76.1   81.8  87.3
             Furametpyr           123572-88-3 C17H20ClN3O2  333.1244   48.3   69.8   86.9   86.2   97.6  101.9
             Fenobucarb           3766-81-2  C12H17NO2     207.1259    60.9   79.2  100.7   96.1  102.8  103.9
             Benodanil            15310-01-7  C13H10INO    322.9807    50.9   69.8   86.3   96.5  102.4  94.8
             Terbuthylazine       5915-41-3  C9H16ClN5     229.1094    50.4   66.6   83.2   87.2   89.8  91.0
             Dimethachlor         50563-36-5  C13H18ClNO2   255.1026   75.1   86.1  106.0  107.1  106.2  108.0
             Dimethenamid         87674-68-8  C12H18ClNO2S  275.0747   72.6   84.9  102.9  100.0  103.6  97.3
             Furalaxyl            57646-30-7  C17H19NO4    301.1314    82.2   89.1  106.6  108.6  106.2  102.4
             Bixafen              581809-46-3 C18H12Cl2F3N3O  413.0310  66.8  79.3   99.0   95.6  103.7  97.1
             Triflumuron          64628-44-0  C15H10ClF3N2O3  358.0332  54.2  71.8   95.5   84.9   95.3  101.7
             Epoxiconazole        133855-98-8 C17H13ClFN3O  329.0731   61.6   77.2   98.8   95.3   90.0  101.2
             Teflubenzuron        83121-18-0  C14H6Cl2F4N2O2  379.9742  41.8  50.9   80.1   86.8  100.0  97.7
   17   18   19   20   21   22   23   24   25   26   27