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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”

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