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Ingredient Analysis                                                                                                       Ingredient Analysis –

                    Hops and Organic Water Contamination                                                                                      Organic Water Contamination



                    Pesticides can be found as contaminants in brewing water and   glyphosate-drenched soil. This example shows results for the   Many common organic water contaminates affecting beer   method USEPA 524 for volatiles* and the liquid injection
                    grains. In particular, the herbicide glyphosate, which has   quantitative determination of glyphosate, glufosinate and    flavor are organic volatile and semi-volatile compounds such as   method USEPA 525 for semi-volatiles. The chromatogram below
                    recently become the focus of the Munich Environmental   AMPA (aminomethylphosphonic acid) using the LCMS-8050             naphthalene, hexachlorobenzene, and                shows the analysis of 76 volatile compounds from 0.5 ppb to 20
                    Institute, has to be monitored carefully since it is probably   triple quadrupole LC/MS/MS system according to DIN 38407-22   hexachlorocyclopentadiene. To analyze these and other specific   ppb. Some countries permit headspace to replace purge and
                    carcinogenic. Elevated concentrations can be expected when   of the German standard methods for the examination of water,   organic compounds in water, follow the purge and trap GCMS   trap methods.
                    glyphosate is applied to a crop shortly before the harvest, a   waste water and sludge. This instrument was used instead of
                    process known as siccation. Siccation is already forbidden in   HPLC with fluorescence detection. The LCMS-8050 allows the
                    Germany and Germany’s farm federation has reconfirmed that   determination of glyphosate in concentrations as low as 0.1   650000  Helium Purge Gas
                    malt derived from glyphosate-sprayed barley has been banned;   µg/L. Sample preparation was done after derivatization with   600000  Nitrogen Purge Gas
                                                                                                                                               550000
                    however, glyphosate could have been used on farms prior to the   9-fluorenylmethyl chloroformate (FMOC-CL).                500000
                                                                                                                                               450000
                    ban, meaning barley could still be grown in                                                                                400000
                                                                                                                                               350000
                                                                                                                                               300000
                                                                                                                                               250000
                               Glyphosate        Perchlorate  Trimesium         Diqaut              Kasugamycine                               200000
                                                                                                                                               150000
                             O       NH 2           O -         CH 3                                    OH                                     100000
                         H 3 C  P         OH     O  Cl  O   H  C  S +  CH       +    +             H O       OH                                50000 0
                             OH                     O        3       3         N    N                                                                  2.5   5.0    7.5   10.0   12.5   15.0
                                       O
                                                                                                   H O       OH                                Overlay of 20 ppb volatile standards purged in helium and nitrogen   Shimadzu GCMS-QP2010 SE Gas Chromatography Mass Spectrometer for
                              Chlormeqaut              Paraquat              ETU                                                               following USEPA method 524                        the Analysis of Volatile and Semi-volatile Compounds
                                                                                             H 3 C  O   O
                                   CH 3                           Cl -                      NH
                                    +                                           NH
                                   N  CH 3    H 3 C  N +         N +  CH 3  H N        H O     NH       NH
                            Cl     CH 3           Cl -                          S         O               2                                   For non-specific organic contaminates, the TOC-L Total Organic   0, 0.3, 0.5, 1, 2, 5, and 10 ppm with a coefficient of
                                  Glufosinate        Mepiquat      Maleic hydrazide    Nicotine         Amitrole                              Carbon analyzer can provide analysis for total organic carbon,   determination (r2) of 0.9996. The TOC-L has an optional
                                                                                                                                              total inorganic carbon, and total carbon by EPA Method 415.3 .   accessory for measuring Total Nitrogen (TN).
                                                                                                                                                                                            #
                                 O      NH 2                          O                H 3 C              N
                             H 3 C  P       OH                                             N                N                                 The 7-point calibration curve shown below includes standards at
                                                         +                                             H N
                                 OH                     N            H N
                                          O
                                                     H 3 C  CH 3       N                                   NH 2
                                                                       H
                                                                           O          N                                                                             Cal. Curve
                                                                                                                                                  45.243
                                                      PTU            Fosethyl aluminium
                                                                                                                                                    40
                                                         NH   S     O    O   CH
                                                H 2 C                H P       3  Al 3+                                                             30
                                                                      O
                                                            NH 2       -
                                                                                 3                                                                 Area  20
                                                                                                                                                    10
                                                                                                                                                    0
                                                                                                                                                      0     2     4     6     8     10  11
                                                                                                                                                                    Cono[mg/L]
                                                                                                                                                    TOC calibration curve from 0-10 ppm in drinking water  Shimadzu TOC-L Total Organic Carbon
                                                                                                                                                                                                          Analyzer for the Analysis of Non-specific Carbon




                                                  Shimadzu LCMS-8050 Triple
                                                  Quadrupole Mass Spectrometer




                    Application News “Highly Polar Pesticide Multi-Residue Analysis in Food Safety by LCMS/MS”                                * Shimadzu Scientific Instruments Application News No. GCMS-1502: “Guide to US EPA Methods 524.3 and 524.4 for Analysis of Volatile Organic Compounds in Drinking Water”
                                                                                                                                              #   Shimadzu Scientific Instruments Application News No. TOC-004: “EPA Method 415.3 - Determination of TOC in Source Water and Drinking Water”

                                                                                                                                                                                         Shimadzu’s Total Support for Beer Analysis
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