natgillin/translations-raw huggingface dataset:
It is essential to examine the appearance of each chromatogram prior to quantitative interpretation, in order to detect any abnormalities due either to malfunctioning of the apparatus or the columns, or to the origin and nature of the sample analysed.
Izračun odzivnih faktorjev R:
If in doubt, repeat the analysis.
R II = odzivni faktorji vrhov II,
Calibration
A II [0] = površine vrhov II standardnega vzorca [0], pridobljene v 8.5.3.
Apply exactly the procedure described from point 8.2 to point 8.4.2 to the standard samples (5.4)
R III = odzivni faktor vrha III,
Use freshly prepared solutions, because CMP degrade in an 8 % trichloroacetic environment.
A III [0] in AIII [5] = površine vrha III standardnega vzorca [0] in [5], pridobljene v 8.5.3,
The loss is estimated at 0,2 % per hour at 30 °C.
W = količina sirotke v standardnem vzorcu [5], tj. 5.
Prior to chromatographic determination of the samples, condition the columns by repeatedly injecting the standard sample (5.4.2) in solution (8.5.1) until the area and retention time of the peak corresponding to the CMP are constant
Izračun relativnih površin vrhov vzorca [E]
Determine the response factors R by injecting the same volume of filtrates (8.5.1) as used for the samples
S II [E], SIII [E], SIV [E] = relativne površine vrhov II, III in IV v vzorcu [E],
EXPRESSION OF RESULTS
A II [E], AIII [E] = površine vrhov II in III v vzorcu [E], pridobljene v 8.4.2,
Method of calculation and formulae
R II, RIII = odzivni faktorji, izračunani v 9.1.1.
Calculation of the response factors R:
Izračun relativnega retenzijskega časa vrha III v vzorcu [E]:
R II = the response factors of peaks II,
RRT III [E] = relativni retenzijski čas vrha III v vzorcu [E],
A II [0] = the areas of peaks II of the standard sample [0] obtained in 8.5.3.
RT III [E] = retenzijski čas vrha III v vzorcu [E], pridobljen v 8.4.2,
R III = the response factor of peak III,
RT III [5] = retenzijski čas vrha III v kontrolnem vzorcu [5], pridobljen v 8.5.3.
A III [0] and AIII [5] = the areas of peak III in standard samples [0] and [5] respectively obtained in 8.5.3,
Preskusi so pokazali, da obstaja linearna povezava med relativnim retenzijskim časom vrha III, npr.
W = the quantity of whey in standard sample [5], i.e. 5.
RRTIII [E], in odstotkom dodane sirotke v prahu do 10 %
Calculation of the relative area of the peaks in the sample [E]
RRTIII [E] je < 1,000, ko je vsebnost sirotke > 5 %,
S II [E], SIII [E], SIV [E] = the relative areas of peaks II, III and IV respectively in the sample [E],
RRTIII [E] je ≥ 1,000, ko je vsebnost sirotke ≤ 5 %.
A II [E], AIII [E] = the areas of peaks II and III respectively in the sample [E] obtained in 8.4.2,
Dovoljena negotovost za vrednosti RRTIII je ± 0,002.
R II, RIII = the response factors calculated in 9.1.1.
Običajno se vrednost RRTIII [0] giblje malo okoli 1,034.
Calculation of the relative retention time of peak III in sample [E]:
Odvisno od stanja kolon se vrednost lahko približa 1,000, ampak mora biti vedno večja od 1,000.
RRT III [E] = the relative retention time of peak III in sample [E],
Izračun deleža sladke sirotke v prahu v vzorcu:
RT III [E] = the retention time of peak III in sample [E] obtained in 8.4.2,
W = SIII[E] – [1, 3 + (SIII[0] – 0, 9)]
RT III [5] = the retention time of peak III in control sample [5] obtained in 8.5.3.
W = odstotek m/m sladke sirotke v vzorcu [E];
Experiments have shown that there is a linear relation between the relative retention time of peak III, i.e.
S III [E] = relativna površina vrha III preskusnega vzorca [E], pridobljena v 9.1.2;
RRTIII [E] and the percentage of whey powder added up to 10 %
1,3 = predstavlja relativno povprečno površino vrha III, izraženo v gramih sladke sirotke na 100 g določene v posnetem mleku v prahu brez primesi različnega izvora.
The RRTIII [E] is < 1,000 when the whey content is > 5 %;
Ta podatek je bil pridobljen eksperimentalno;
The RRTIII [E] is ≥ 1,000 when the whey content is ≤ 5 %.
S III [0] = predstavlja relativno površino vrha III, ki je enaka RIII × AIII [0].
The uncertainty allowed for the values of RRTIII is ± 0,002.
Te vrednosti so pridobljene v 9.1.1 in 8.5.3;
Normally the value of RRTIII [0] deviates little from 1,034.
(S III [0] – 0,9) = predstavlja popravek za relativno povprečno površino 1,3, ko SIII [0] ni enako 0,9.
Depending on the condition of the columns, the value may approach 1,000, but it shall always be greater.
Eksperimentalno je relativna povprečna površina vrha III kontrolnega vzorca [0] 0,9.
Calculation of the percentage of rennet whey powder in the sample:
Zanesljivost postopka
W = SIII[E] – [1, 3 + (SIII[0] – 0,9)]
Razlika med rezultatoma dveh določitev, ki ju izvede simultano ali po kratkem času isti analitik z isto opremo in na enakem preskusnem materialu, ne sme presegati 0,2 % m/m.
W = the percentage m/m of rennet whey in the sample [E];
Razlika med dvema posamičnima in neodvisnima rezultatoma, dobljenima v dveh različnih laboratorijih na enakem preskusnem materialu, ne sme presegati 0,4 % m/m.
S III [E] = the relative area of peak III of test sample [E] obtained as in 9.1.2;
Interpretacija
1,3 = represents the relative average area of peak III expressed in grams of rennet whey per 100 g determined in non-adulterated skimmed milk powder of various origins.
Če je relativna površina vrha III, SIII [E], izražena v gramih sladke sirotke na 100 g proizvoda ≤ 2,0 + (SIII[0] – 0,9), je treba zanikati obstoj sirotke,
This figure was obtained experimentally;
kjer je:
S III [0] = represents the relative area of peak III which is equal to RIII × AIII [0].
največja dovoljena vrednost relativne površine vrha III ob upoštevanju relativne povprečne površine vrha III, npr. 1,3, negotovosti zaradi sprememb v sestavi posnetega mleka v prahu in obnovljivosti metode (9.3.2);
These values are obtained in 9.1.1 and 8.5.3 respectively;
popravek, ki ga je treba upoštevati, ko se površina SIII [0] razlikuje od 0,9 (glej točko 9.2).
(S III [0] – 0,9) = represents the correction to be made to the relative average area 1,3 when SIII [0] is not equal to 0,9.
Če je relativna površina vrha III, SIII [E] > 2,0 + (SIII[0] – 0,9) in relativna površina vrha II, SII [E] ≤ 160, določite vsebnost sladke sirotke, kot je navedeno v točki 9.2.
Experimentally the relative average area of peak III of the control sample [0] is 0,9.
Če je relativna površina vrha III, SIII [E] > 2,0 + (SIII[0] – 0,9) in relativna površina vrha II, SII [E] ≤ 160, določite vsebnost skupnih beljakovin (P %); nato preučite grafa 1 in 2.
Accuracy of the procedure
Podatki, dobljeni po analizi nepotvorjenih vzorcev posnetega mleka v prahu z visoko vsebnostjo skupnih beljakovin, so zbrani v grafih 1 in 2.
The difference between the results of two determinations carried out simultaneously or in rapid succession by the same analyst using the same apparatus on identical test material shall not exceed 0,2 % m/m.
Neprekinjena črta predstavlja linearno regresijo, katere koeficienti so izračunani z metodo najmanjših kvadratov.
The difference between two single and independent results, obtained in two different laboratories on identical test material shall not exceed 0,4 % m/m.
Prekinjena ravna črta označuje zgornjo mejo relativne površine vrha III z verjetnostjo, da v 90 % primerov ni presežena.
Interpretation
Enačbi prekinjenih ravnih črt v grafih 1 in 2 sta:
Assume the absence of whey if the relative area of peak III, SIII [E] expressed in grams of rennet whey per 100 g of the product is ≤ 2,0 + (SIII[0] – 0,9)
(graf 1),
where
(graf 2),
is the maximum value allowed for the relative area of peak III taking into account the relative average area of peak III, i.e. 1,3, the uncertainty due to variations in the composition of skimmed milk powder and the reproducibility of the method (9.3.2),
kjer je:
is the correction to be made when the area SIII [0] is different from 0,9 (see point 9.2)
relativna površina vrha III, izračunana bodisi v skladu z vsebnostjo skupnih beljakovin bodisi v skladu z relativno površino vrha SII [E],
If the relative area of peak III, SIII [E] is > 2,0 + (SIII[0] – 0,9) and the relative area of peak II, SII [E] ≤ 160, determine the rennet whey content as indicated in point 9.2.
P % vsebnost skupnih beljakovin, izražena v masnih odstotkih,
If the relative area of peak III, SIII [E] is > 2,0 + (SIII[0] – 0,9) and the relative area of peak II, SII [E] ≤ 160, determine the total protein content (P %); then examine graphs 1 and 2.
relativna površina vzorca, izračunana v točki 9.1.2.
The data obtained after analysis of samples of unadulterated skimmed milk powders with a high total protein content have been assembled in graphs 1 and 2.
Te enačbe so enakovredne vrednosti 1,3, navedeni v točki 9.2.
The continuous line represents the linear regression, the coefficients of which are calculated by the least squares method.
Odstopanje (T1 in T2) med relativno površino SIII [E] in relativno površino SIII je prikazano z naslednjimi vrednostmi: T1 = SIII[E] – [(0,376 P% - 10,7) + (SIII[0] – 0,9)]T2 = SIII[E] – [(0,0123 SII[E] + 0,93) + (SIII[0] – 0,9)]
The dashed straight line fixes the upper limit of the relative area of peak III with a probability of not being exceeded in 90 % of cases.
Če je T1 in/ali T2
The equations for the dashed straight lines of graphs 1 and 2 are:
nič ali manj, prisotnosti sladke sirotke ni mogoče določiti.
(graph 1),
Če sta T1 in T2
(graph 2),
večji kot nič, je sladka sirotka prisotna.
respectively where:
Vsebnost sladke sirotke se izračuna v skladu z naslednjo enačbo: W = T2 + 0,91
is the relative area of peak III calculated either according to total protein content or according to the relative area of peak SII [E],
0,91 razdalja navpičnih osi med neprekinjenimi in pikčastimi ravnimi črtami.
P % is the total protein content expressed as a percentage, by weight,
Vrh II
is the relative area of sample calculated in point 9.1.2.
Posneto mleko v prahu
These equations are equivalent to the figure of 1,3 mentioned in point 9.2.
Skupna vsebnost beljakovin (%)
The discrepancy (T1 and T2) between the relative area SIII [E] found and the relative area SIII is given by means of the following: T1 = SIII[E] – [(0,376 P% – 10,7) + (SIII[0] – 0,9)]T2 = SIII[E] – [(0,0123 SII[E] + 0,93) + (SIII[0] – 0,9)]
Vrh III
If T1 and/or T2
Dodatek III
are zero or less, the presence of rennet whey cannot be determined.
DOLOČANJE TRDNIH SNOVI SLADKE SIROTKE V POSNETEM MLEKU V PRAHU
If T1 and T2
NAMEN: ZAZNAVANJE DODATKA TRDNIH SNOVI SLADKE SIROTKE K POSNETEMU MLEKU V PRAHU
exceed zero, rennet whey is present.
SKLICI: MEDNARODNI STANDARD ISO 707
The rennet whey content is calculated according to the following formula: W = T2 + 0,91
Vsebnost trdnih snovi sladke sirotke je opredeljena kot masni odstotek, ki se določi z vsebnostjo makropeptidov kazeina v skladu z opisanim postopkom.
0,91 is the distance on the vertical axis between the continuous and dotted straight lines.
Pri vzorcih se analizira vsebnost makropeptida kazeina A s tekočinsko kromatografijo visoke ločljivosti z reverzno fazo (HPLC-postopek).
Peak II
Rezultati se ocenijo glede na standardne vzorce posnetega mleka v prahu z znanim deležem in brez znanega deleža sirotke v prahu.
Skimmed milk powder
Rezultati, ki presegajo 1 % masnega deleža, kažejo na prisotnost trdnih snovi sladke sirotke.
total protein content (%)
Kakovost acetonitrila mora biti primerna za spektroskop ali HPLC.
Peak III
Eluenta A in B
Appendix III
Eluent A: V 1000-mililitrsko merilno bučko dodajte 150 ml acetonitrila (CH3CN), 20 ml izopropanola (CH3CHOHCH3) in 1,00 ml trifluoroocetne kisline (TFA, CF3COOH).
DETERMINING RENNET WHEY SOLIDS IN SKIMMED MILK POWDER
Dopolnite z vodo do 1000 ml.
PURPOSE: DETECTING THE ADDITION OF RENNET WHEY SOLIDS TO SKIMMED MILK POWDER
Dopolnite z vodo do 1000 ml.
The content of rennet whey solids is defined as the percentage by mass as determined by caseinomacropeptide content by the procedure described.
Po analizi kolono sperete z eluentom B (gradientno) in potem še z acetonitrilom (gradientno v 30 minutah.).
Samples are analysed for caseinomacropeptide A by a reversed-phase high-performance liquid chromatography procedure (HPLC procedure).
Kolona se shrani v acetonitrilu.
Evaluation of the result is obtained by reference to standard samples consisting of skimmed milk powder with and without a known percentage of whey powder.
Posneto mleko v prahu, ki ustreza zahtevam za javno skladiščenje (npr. [0]).
Results higher than 1 % (m/m) show that rennet whey solids are present.
Enako posneto mleko v prahu z dodatkom 5 % (m/m) sladke sirotke v prahu s standardno sestavo (tj. [5]).
Acetonitrile should be of spectroscopic or HPLC quality.
Enako posneto mleko v prahu z dodatkom 50 % (m/m) sladke sirotke v prahu s standardno sestavo (tj. [50]).
Eluents A and B
Graduirana pipeta, ki prepušča 10 ml (ISO 648, razred A, ali ISO/R 835) ali razdelilni sistem, ki lahko prepušča 10,0 ml v dveh minutah
Eluent A: 150 ml of acetonitrile (CH3CN), 20 ml of isopropanol (CH3CHOHCH3), and 1,00 ml of trifluoroacetic acid (TFA, CF3COOH) are placed in a 1000 ml volumetric flask.
Binarni gradientni sistem črpalk
Make up to 1000 ml with water.
Ročni ali avtomatski injektor s prostornino 100 μl
Eluent B: 550 ml of acetonitrile, 20 ml of isopropanol and 1,00 ml of TFA are placed in a 1000 ml volumetric flask.
Kolona Agilent Technologies Zorbax 300 SB-C3 (dolžina 25 cm, notranji premer 0,46 cm) ali enakovredna silicijeva kolona s širokimi porami za reverzno kromatografijo
Conservation of the column
UV-detektor z nastavljivo valovno dolžino in z možnostjo merjenja pri 210 nm (če je potrebno, se lahko uporabi višja valovna dolžina do 220 nm) z občutljivostjo 0,02 Å
After the analyses the column is flushed with eluent B (via a gradient) and subsequently flushed with acetonitrile (via a gradient for 30 minutes).
Integrator, ki lahko določi integracijo na splošni bazni liniji ali dolina–dolina
The column is stored in acetonitrile.
Opomba: Delo s kolonami je mogoče tudi pri sobni temperaturi, če temperatura niha manj kot ± 1 °C, sicer nastane preveliko nihanje retenzijskega časa CMPA.
Skimmed milk powder meeting the requirements for public storage (i.e. [0]).
Vzorec hranite pri pogojih, ki izključujejo kakršno koli kvarjenje ali spremembo sestave.
The same skimmed milk powder adulterated with 5 % (m/m) rennet-type whey powder of standard composition (i.e. [5]).
Odtehtajte 2,00 ± 0,001 g preskusnega vzorca v epruveto za centrifugiranje (6.2) ali ustrezno zaprto bučko (50 ml).
The same skimmed milk powder adulterated with 50 % (m/m) rennet-type whey powder of standard composition (i.e. [50])
Opomba: V primeru mešanic odtehtajte takšno količino preskusnega vzorca, da razmaščeni vzorec deleža ustreza 2,00 g.
Graduated pipettes, allowing delivery of 10 ml (ISO 648, Class A, or ISO/R 835), or a dispensing system capable of delivering 10,0 ml in two minutes
V dveh minutah dodajte 10,0 ml raztopine triklorocetne kisline s temperaturo približno 25 °C (5.1) in pri tem intenzivno mešajte z magnetnim mešalnikom (6.4).
Binary gradient pumping system
Centrifugirajte (6.2) 10 minut pri 2200 g ali filtrirajte skozi filter (6.6) in zavrzite prvih 5 ml filtrata.
Injector, hand or automatic, with a 100 μl capacity
Metoda HPLC na reverzni fazi izključuje možnost lažno pozitivnih rezultatov zaradi prisotnosti kislega pinjenca v prahu.
Agilent Technologies Zorbax 300 SB-C3 column (length 25 cm, 0,46 cm internal diameter) or an equivalent wide-pore silica based reversed-phase column
Pred izvedbo HPLC-analize na reverzni fazi je treba optimizirati gradientne pogoje.
Variable wavelength UV detector, permitting measurements at 210 nm (if necessary, a higher wavelength up to 220 nm may be used) with a sensitivity of 0,02 Å
Retenzijski čas CMPA 26 ± 2 minuti je optimalen za gradientne sisteme z mrtvo prostornino približno 6 ml (prostornina od točke, na kateri pridejo skupaj topila, do vključno s prostornino injekcijske zanke).
Integrator capable of setting the integration to common baseline or valley-to-valley
Gradientni sistemi z manjšo mrtvo prostornino (npr. 2 ml) naj uporabijo 22 minut kot optimalen retenzijski čas.
Note: Operation of the column at room temperature is possible, provided that the room temperature does not fluctuate more than 1 °C, otherwise too much variation in the retention time of CMPA takes place.
Odvzem raztopine standardnih vzorcev (5.4) brez sladke sirotke in s 50 % sladke sirotke.
Store the sample in conditions which preclude any deterioration or change in composition.
Vbrizgajte 100 μl supernatanta ali filtrata (8.3.3) v instrument HPLC, ki deluje pri predlaganih gradientnih pogojih, danih v tabeli 1.
Weigh 2,00 ± 0,001 g of test sample into a centrifuge tube (6.2) or suitable stoppered flask (50 ml).
Tabela 1
Note: In the case of mixtures, weigh such an amount of the test sample that the defatted sample portion corresponds to 2,00 g.
Predlagani gradientni pogoji za optimizacijo kromatografije
Add 10,0 ml of the trichloroacetic acid solution of ca.
Čas
25 °C (5.1) constantly over two minutes, while stirring vigorously with the aid of the magnetic stirrer (6.4).
Pretok
Centrifuge (6.2) 2200 g for 10 minutes, or filter through paper (6.6), discarding the first 5 ml of filtrate
Krivulja
The reversed-phase HPLC method excludes the possibility false-positive results due to the presence of acid buttermilk powder.
linearna
Before the reversed phase HPLC-analysis is carried out, the gradient conditions should be optimised.
Iz primerjave dveh kromatogramov se razbere lokacija vrha CMPΑ.
A retention time of 26 ± 2 minutes for CMPA is optimal for gradient systems having a dead volume of about 6 ml (volume from the point where the solvents come together to the volume of the injector loop, inclusive).
Po navedeni enačbi se lahko izračuna sestava začetnega topila, ki se uporabi za normalni gradient (glej 8.4.3): % B = 10 – 2,5 + (13,5 + (RTcmpA – 26) / 6)*30 / 27 % B = 7,5 + (13,5 + (RTcmpA – 26) / 6)*1,11,
Gradient systems having a lower dead volume (e.g. 2 ml) should use 22 minutes as an optimal retention time
kjer je:
Take solutions of the standard samples (5.4) without and with 50 % rennet whey.
RT cmpA : retenzijski čas CMPΑ v predlaganem gradientu
Inject 100 μl of supernatant or filtrate (8.3.3) into the HPLC apparatus operating at the scouting gradient conditions given in Table 1.
10 : začetni % B v predlaganem gradientu
Table 1
2,5 : % B na sredini minus % B na začetku normalnega gradienta
Scouting gradient conditions for optimisation of the chromatography
13,5 : srednji čas predlaganega gradienta
Time
26 : zahtevani retenzijski čas CMPΑ
Flow
6 : razmerje naklonov predlaganega in normalnega gradienta
Curve
30 : % B na začetku minus % B pri 27 minutah predlaganega gradienta
linear
27 : celotni čas predlaganega gradienta.
Comparison of the two chromatograms should reveal the location of the peak of CMPΑ.
Odvzem raztopin preskusnih vzorcev
Using the formula given below, the initial solvent composition to be used for the normal gradient (see 8.4.3) can be calculated % B = 10 – 2,5 + (13,5 + (RTcmpA – 26) / 6) * 30 / 27 % B = 7,5 + (13,5 + (RTcmpA – 26) / 6) * 1,11
Vbrizgajte 100 μl natančno odmerjenega supernatanta ali filtrata (8.3.3) v instrument HPLC, ki deluje pri pretoku 1,0 ml raztopine eluenta (5.2) na minuto.
Where:
Sestavo eluenta na začetku analize dobite iz 8.4.2.
RT cmpA : retention time of CMPΑ in the scouting gradient
Ponavadi je blizu A:B = 76:24 (5.2).
10 : the initial % B of the scouting gradient
Takoj po vbrizgavanju se vklopi linearni gradient, ki ima po 27 minutah za 5 % višji delež B.
2,5 : % B at midpoint minus % B at initial in the normal gradient
Nato se vklopi linearni gradient, ki v petih minutah spremeni sestavo eluenta na 90 % B.
13,5 : midpoint time of the scouting gradient
Ta sestava se ohrani pet minut, potem pa se prek linearnega gradienta v petih minutah spremeni v začetno sestavo.
26 : required retention time of CMPΑ
Odvisno od notranje prostornine sistema črpalk lahko naslednje vbrizgavanje sledi 15 minut zatem, ko dosežete začetno sestavo.
6 : ratio of slopes of the scouting and normal gradient
To je mogoče doseči s spreminjanjem začetnih in končnih pogojev prvega gradienta.
Take solutions of the test samples
Standardni odmik retenzijskega časa CMPA vrha naj bo manjši od 0,1 minute (n = 10).
Inject 100 μl of accurately measured supernatant or filtrate (8.3.3) into the HPLC apparatus operating at a flow rate of 1,0 ml of eluent solution (5.2) per minute.
Rezultati kromatografske analize preskusnega vzorca (E) so dobljeni v obliki kromatograma, v katerem je vrh CMPA prepoznan z retenzijskim časom približno 26 minut.
Immediately after the injection a linear gradient is started, which results in a 5 % higher percentage of B after 27 minutes.
Analizo ali integracijo je treba ponoviti, če je bazna linija nepravilno določena.
Subsequently a linear gradient is started, which brings the eluent composition to 90 % B in five minutes.
Opomba: Če je vrh CMPA dovolj ločen od drugih vrhov, je treba uporabiti bazno linijo dolina–dolina, v nasprotnem primeru uporabite padajoče navpičnice za splošno bazno linijo, ki mora imeti izhodišče blizu vrha CMPA (torej ne pri t = 0 min!).Za standard in vzorec uporabite enako vrsto integracije in v primeru splošne bazne linije preverite skladnost vrste za vzorce in standard.
Note 1.
Uporabite sveže pripravljene raztopine, ker se CMP razgradi v 8-odstotni triklorocetni kislini pri sobni temperaturi.
The retention time of the CMPA should be 26 ± 2 minutes.
Pri 4 °C ostane raztopina stabilna 24 ur.
This can be achieved by varying the initial and end conditions of the first gradient.
Pri veliki seriji analiz je zaželena uporaba hlajenega pladnja za vzorce v avtomatskem injektorju.
However, the difference in the % B for the initial and end conditions of the first gradient shall remain 5 % B.
Opomba: Točko 8.4.2 je mogoče izpustiti, če je % B pri začetnih pogojih znan iz prejšnjih analiz.
Note 2.
Kromatogram referenčnega vzorca [5] mora biti analogen sliki 1.
The eluents should be degassed sufficiently and should also remain degassed.
Na tej sliki sta pred vrhom CMPA dva majhna vrhova.
This is essential for proper functioning of the gradient pumping system.
Nujno je, da dobite podobno ločevanje.
The standard deviation for the retention time of the CMPA peak should be smaller than 0,1 minutes (n = 10).
Pred kromatografskim določanjem vzorcev vbrizgajte 100 μl standardnega vzorca brez sladke sirotke [0] (5.4.1).
Note 3.
Kromatogram ne sme imeti vrha pri retenzijskem času vrha CMPA.
Every five samples the reference sample [5] should be injected and used to calculate a new response factor R. (9.1.1).
Z vbrizganjem enake prostornine filtrata (8.5.1), kakor je uporabljen pri vzorcih, določite odzivne faktorje R.
The results of the chromatographic analysis of the test sample (E) are obtained in the form of a chromatogram in which the CMPA peak is identified by its retention time of about 26 minutes
Izračun odzivnega faktorja R:
The integrator (6.11.6) automatically calculates the peak height H of the CMPA peak.
vrh CMPA: R = W/H,
The baseline location should be checked in every chromatogram.
R = R odzivni faktor vrha CMPA,
The analysis or the integration should be repeated if the baseline was incorrectly located.
H = višina vrha CMPA,
Note: If the CMPA peak is sufficiently separated from other peaks valley-to-valley baseline allocation should be used, otherwise use dropping perpendiculars to a common baseline, which should have starting point close to the CMPA peak (thus not at t = 0 min!).Use for the standard and the samples the same type integration type and check in case of common baseline its consistency for the samples and the standard.
W = količina sirotke v standardnem vzorcu [5].
It is essential to examine the appearance of each chromatogram prior to quantitative interpretation, in order to detect any abnormalities due either to malfunctioning of the apparatus or the column, or to the origin and nature of the sample analysed.
Izračun deleža sladke sirotke v prahu v vzorcu
Apply exactly the procedure described from point 8.2 to point 8.4.4 to the standard samples (5.4.1 to 5.4.2).
W(E) = odstotek (m/m) sladke sirotke v vzorcu (E);