Page 49 - Application Notebook - Solution for Food Safety
P. 49

Application   No. C161
    News


            „  Quantitation Results using MRM Spectrum Mode
            To assess the robustness of the MRM Spectrum mode,   compared to those of the MRM Spectrum mode (Fig. 4).
            the same sample was repeatedly injected. The method   Both methods resulted in a variance of less than
            used complies with the identification criteria set out in   4 %RSD (n=10 for each method; 10 pg/uL spiked into
            the EU guidelines SANTE/11945/2015 that require the   salmon matrix). Fig. 5 indicates MRM spectra and the
            retention time and the ion ratio from at least 2 MRM ion   calibration curve obtained for sulfamerazine as an
            ratios to be  within acceptable tolerance limits. The   example of quantitation results.
            absolute response and signal  variability were


                                            156.05
                    8.89e5
                        Sulfamerazine
                        1 pg/μL    92.05108.05                               Compound name Sulfamerazine
                        Matrix  Beef          172.05                         Precursor 265.10 [M+H]+
                                       110.05
                                65.00                                        Formula C11H12N4O2S
                                                                             CAS 127-79-7
                                  80.05
                            38.95  66.05  93.10   199.10
                                                                                    N  O  O
                       0  20  40  60  80  100 120 140 160 180  m/z
                    8.49e6                  156.05                                      S
                        Sulfamerazine                                      H 3 C  N   NH
                        100 pg/μL   92.05 108.05  172.05
                        Matrix  Beef
                                65.00  110.05                                                     NH 2
                                  80.05
                            38.95  66.05  93.10   199.10
                       0  20  40  60  80  100 120 140 160 180  m/z        MRM Spectrum Mode
                                                                          11 MRM’s acquired for sulfamerazine in beef.
                       4.5  Sulfamerazine                                 1:265.10>156.05 (+)  CE: -17V
                        4  Calibration curve 1-                           2:265.10>92.05 (+)  CE: -30V
                       3.5  100 pg/μL                                     3:265.10>172.05 (+)  CE: -15V
                        3  Matrix  Beef                                   4:265.10>108.05 (+)  CE: -26V
                                                                          5:265.10>65.00 (+)
                                                                                          CE: -11V
                       2.5                                                6:265.10>110.05 (+)  CE: -22V
                        2                                                 7:265.10>80.05 (+)  CE: -15V
                       1.5                                                8:265.10>38.95 (+)  CE: -14V
                        1                 y = 0.0419x + 0.0085            9:265.10>199.10 (+)  CE: -21V
                       0.5                  R² = 0.9997                   10:265.10>93.10 (+)  CE: -30V
                                                                                          CE: -24V
                                                                          11:265.10>66.05 (+)
                        0
                         0   20   40   60   80  100
                                                             5.60  5.70 min
                                  Concentration
                                  (pg/uL)

                                    MRM Spectra and Calibration Curve of Sulfamerazine (1 pg/μL to 100 pg/μL)


            „  Conclusion
            The level of confidence in compound identification and   generation of a high quality product ion spectrum
            verification was increased by using a higher number of   which can  be used to achieve  highly reliable
            MRM transitions for  each veterinary drug target and   compound identification and verification by library
            thereby reducing false negative and false positive   searching. In this research, use of the MRM Spectrum
            reporting. Although the number of transitions for each   mode was  examined by quantifying and identifying
            target is dependent upon the chemical structure of the   212 veterinary drugs (the method included 2,009 MRM
            target, typically more than 10 transitions can be   transitions). Limits of detection, linearity or
            monitored for each compound. MRM Spectrum mode     repeatability were not compromised compared to a
            combines conventional quantitation with the        conventional 2-MRM method.











                                                                                                      First Edition: Aug. 2017
                                             For Research Use Only. Not for use in diagnostic procedure.
                                             This publication may contain references to products that are not available in your country. Please contact us to check the availability of these
                                             products in your country.

                                             The content of this publication shall not be reproduced, altered or sold for any commercial purpose without the written approval of Shimadzu.
                                             Company names, product/service names and logos used in this publication are trademarks and trade names of Shimadzu Corporation or its
                                             affiliates, whether or not they are used with trademark symbol “TM” or “£”. Third-party trademarks and trade names may be used in this
                                             publication to refer to either the entities or their products/services. Shimadzu disclaims any proprietary interest in trademarks and trade names
     www.shimadzu.com/an/                    other than its own.

                                             The information contained herein is provided to you "as is" without warranty of any kind including without limitation warranties as to its
                                             accuracy or completeness. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the
                                             use of this publication. This publication is based upon the information available to Shimadzu on or before the date of publication, and subject
                                             to change without notice.
                                                                                                  © Shimadzu Corporation, 2017
   44   45   46   47   48   49   50   51   52   53   54