In anaerobicdigestionoforganicmatter,severalmetabolicpathwaysareinvolvedduringthesimulta-
neous productionandconsumptionofshort-chainfattyacids(SCFA)ingeneralandacetateinparticular.
Understandingtheroleofeachpathwayrequiresboththedeterminationoftheconcentrationandiso-
tope enrichmentofintermediatesinconjunctionwithisotopelabeledsubstrates.Theobjectiveofthis
study wastoestablisharapidandsimpleGC/MSmethodfordeterminingtheisotopeenrichmentof
acetate andconcentrationofunderivatizedshort-chainfattyacids(SCFA)inbiogasdigestersamplesby
direct liquidinjectionofacidified aqueoussamples.Samplepreparationinvolvesonlyacidification,
centrifugation and filtration oftheaqueoussolutionfollowedbydirectinjectionoftheaqueoussuper-
natant solutionontoapolarcolumn.WiththesamplepreparationandGC/MSconditionsemployed,
well-resolvedandsharppeaksofunderivatizedSCFAwereobtainedinareasonablyshorttime.Good
recovery(96.6–102.3%)aswellaslowdetection(4–7 mmol/L) andquantification limits(14–22 mmol/L)
wereobtainedforallthe6SCFAstudied.Goodlinearitywasachievedforbothconcentrationandisotope
enrichment measurementwithregressioncoefficients higherthan0.9978and0.9996,respectively.The
method hasagoodintra-andinter-dayprecisionwitharelativestandarddeviation(RSD)below6%for
determining thetracer-to-traceeratio(TTR)ofboth[2-13C]acetate and[U-13C]acetate.Ithasalsoagood
intra– and inter-dayprecisionwithaRSDbelow6%and5%fordeterminingtheconcentrationofstandard
solution andbiogasdigestersamples,respectively.Acidification ofbiogasdigestersampleswithoxalic
acid providedthelowpHrequiredfortheprotonationofSCFAandthus,allowstheextractionofSCFA
from thecomplexsamplematrix.Moreover,oxalicacidwasthesourceofformicacidwhichwaspro-
duced intheinjectorsetathightemperature.TheproducedformicacidpreventedtheadsorptionofSCFA
in thecolumn,therebyeliminatingpeaktailingandghostpeaks.TheapplicabilityofthevalidatedGC/MS
method fordeterminingtheconcentrationofacetateandits 13C isotopeenrichmentinanaerobicdigester
samples wastestedandtheresultsdemonstratedthesuitabilityofthismethodforidentifyingthe
metabolic pathwaysinvolvedindegradationandproductionofacetate.
ใน anaerobicdigestionoforganicmatter, severalmetabolicpathwaysareinvolvedduringthesimulta-
neous enrichmentofintermediatesinconjunctionwithisotopelabeledsubstrates.Theobjectiveofthis ศึกษา wastoestablisharapidandsimpleGC / MSmethodfordeterminingtheisotopeenrichmentof acetate andconcentrationofunderivatizedshort-chainfattyacids (SCFA) inbiogasdigestersamplesby โดยตรง liquidinjectionofacidified aqueoussamples.Samplepreparationinvolvesonlyacidification, ปั่นและกรอง oftheaqueoussolutionfollowedbydirectinjectionoftheaqueoussuper- natant มิลลิโมล / ลิตร) andquantification ข้อ จำกัด (14-22 measurementwithregressioncoefficients higherthan0.9978and0.9996, ตามลำดับวิธีการhasagoodintra-andinter-dayprecisionwitharelativestandarddeviation (RSD) below6% สำหรับการกำหนดthetracer ไป traceeratio (TTR) ofboth [2-13C] อะซิเตทและ [U-13C] acetate.Ithasalsoagood intra- และ ระหว่าง dayprecisionwithaRSDbelow6% and5% fordeterminingtheconcentrationofstandard andbiogasdigestersamples โซลูชั่น respectively.Acidification ofbiogasdigestersampleswithoxalic กรด providedthelowpHrequiredfortheprotonationofSCFAandthus, allowstheextractionofSCFA จาก thecomplexsamplematrix.Moreover, oxalicacidwasthesourceofformicacidwhichwaspro- โฉม intheinjectorsetathightemperature.TheproducedformicacidpreventedtheadsorptionofSCFA ใน thecolumn, therebyeliminatingpeaktailingandghostpeaks.TheapplicabilityofthevalidatedGC / MS วิธี fordeterminingtheconcentrationofacetateandits 13C isotopeenrichmentinanaerobicdigester ตัวอย่าง wastestedandtheresultsdemonstratedthesuitabilityofthismethodforidentifyingthe pathwaysinvolvedindegradationandproductionofacetate การเผาผลาญอาหาร
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ใน anaerobicdigestionoforganicmatter severalmetabolicpathwaysareinvolvedduringthesimulta , -
neous productionandconsumptionofshort chainfattyacids ( scfa ) ingeneralandacetateinparticular .
understandingtheroleofeachpathwayrequiresboththedeterminationoftheconcentrationandiso enrichmentofintermediatesinconjunctionwithisotopelabeledsubstrates theobjectiveofthis
-
tope .การศึกษา wastoestablisharapidandsimplegc / msmethodfordeterminingtheisotopeenrichmentof
อะซิเตท andconcentrationofunderivatizedshort chainfattyacids ( scfa ) inbiogasdigestersamplesby
ตรง liquidinjectionofacidified aqueoussamples . samplepreparationinvolvesonlyacidification
ปั่นและกรอง , oftheaqueoussolutionfollowedbydirectinjectionoftheaqueoussuper -
natant solutionontoapolarcolumn .withthesamplepreparationandgc / msconditionsemployed
resolvedandsharppeaksofunderivatizedscfawereobtainedinareasonablyshorttime , ดี ดี
Recovery ( 96.6 – 102.3 % ) aswellaslowdetection ( 4 – 7 mmol / L ) andquantification จำกัด ( 14 – 22 mmol / L )
wereobtainedforallthe6scfastudied . goodlinearitywasachievedforbothconcentrationandisotope เสริม higherthan0.9978and0.9996 measurementwithregressioncoefficients ,โดย
วิธี hasagoodintra andinter dayprecisionwitharelativestandarddeviation ( RSD ) below6 %
กำหนด thetracer เพื่อ traceeratio ( TTR ) ของ [ ] [ ] 2-13c อะซิเตท และ u-13c อะซิเทต และภายใน ithasalsoagood
inter-dayprecisionwitharsdbelow6 % และ 5 % fordeterminingtheconcentrationofstandard และโซลูชั่น andbiogasdigestersamples respectively.acidification ofbiogasdigestersampleswithoxalic
,กรด providedthelowphrequiredfortheprotonationofscfaandthus allowstheextractionofscfa
, จาก thecomplexsamplematrix นอกจากนี้ oxalicacidwasthesourceofformicacidwhichwaspro -
duced intheinjectorsetathightemperature . theproducedformicacidpreventedtheadsorptionofscfa ใน thecolumn
,
theapplicabilityofthevalidatedgc / MS therebyeliminatingpeaktailingandghostpeaks .วิธี fordeterminingtheconcentrationofacetateandits 13C isotopeenrichmentinanaerobicdigester
ตัวอย่าง wastestedandtheresultsdemonstratedthesuitabilityofthismethodforidentifyingthe สลาย pathwaysinvolvedindegradationandproductionofacetate .
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