natgillin/translations-raw huggingface dataset:
The extract is dried and an aliquot portion subjected to a clean-up on an aluminium oxide column.
Ekstrakt se osuši in alikvot se prečisti na koloni iz aluminijevega oksida.
Robenidine is eluted from the column with methanol, concentrated, and made up to a suitable volume with mobile phase.
Robenidin se eluira s kolone z metanolom, koncentrira in dopolni z mobilno fazo do ustreznega volumna.
The content of robenidine is determined by reversed-phase high-performance liquid chromatography (HPLC) using an UV detector.
Vsebnost robenidina se določi s tekočinsko kromatografijo visoke ločljivosti (HPLC) z reverzno fazo in UV-detektorjem.
Acidified methanol.
Nakisani metanol
Transfer 4,0 ml hydrochloric acid (ρ20 = 1,18 g/ml) into a 500 ml graduated flask, make up to the mark with methanol (3.1) and mix.
4,0 ml klorovodikove kisline (ρ20 = 1,18 g/ml) se prenese v 500-mililitrsko merilno bučko, dopolni se do oznake z metanolom (3.1) in premeša.
This solution shall be freshly prepared before use.
Ta raztopina se pred vsako uporabo sveže pripravi.
Molecular sieve.
Molekularno sito
Type 3A, 8 to 12 mesh beads (1,6-2,5 mm beads, crystalline alumino-silicate, diameter of pores 0,3 mm).
Tip 3A, kroglice 8 do 12 meš (kroglice, premera 1,6 – 2,5 mm, kristalinični aluminijev silikat, premer por 0,3 mm)
Aluminium oxide acidic activity grade I for column chromatography.
Stopnja kislinske aktivnosti I aluminijevega oksida, za kolonsko kromatografijo
Transfer 100 g aluminium oxide into a suitable container and add 2,0 ml of water.
V primerno posodo se prenese 100 g aluminijevega oksida in doda 2,0 ml vode.
Potassium dihydrogen phosphate solution, c = 0,025 mol/l.
Raztopina kalijevega dihidrogenfosfata, c = 0,025 mol/l
Dissolve 3,40 g of potassium dihydrogen phosphate in water (HPLC grade) in a 1000 ml graduated flask, make up to the mark and mix.
3,40 g kalijevega dihidrogenfosfata se raztopi v vodi (za HPLC) v 1000-mililitrski merilni bučki, dopolni se do oznake in premeša.
Di-sodium hydrogen phosphate solution, c = 0,025 mol/l.
Raztopina dinatrijevega hidrogenfosfata, c = 0,025 mol/l
Dissolve 3,55 g of anhydrous (or 4,45 g of dihydrate or 8,95 g of dodecahydrate) di-sodium hydrogen phosphate in water (equivalent to HPLC grade) in a 1 litre graduated flask, make up to the mark and mix.
3,55 g brezvodnega dinatrijevega hidrogenfosfata (ali 4,45 g dihidrata ali 8,95 g dodekahidrata) se raztopi v vodi (za HPLC) v 1000-mililitrski merilni bučki, dopolni se do oznake in premeša.
HPLC mobile phase.
HPLC-mobilna faza
Mix together the following reagents:
Zmešajo se naslednji reagenti:
650 ml acetonitrile (3.3),
650 ml acetonitrila (3.3),
250 ml water (equivalent to HPLC-grade),
250 ml vode (za HPLC),
50 ml potassium di-hydrogen phosphate solution (3.6),
50 ml raztopine kalijevega dihidrogenfosfata (3.6),
50 ml di-sodium hydrogen phosphate solution (3.7).
50 ml raztopine dinatrijevega hidrogenfosfata (3.7).
Filter through a 0,22 μm filter (4.6) and degas the solution, (e.g. by ultrasonification for 10 minutes).
Filtrira se skozi filter 0,22 μm (4,6), raztopina pa se nato razplini (npr. 10 minut v ultrazvočni kopeli).
Standard substance.
Standardna snov
Pure robenidine: 1,3-bis [(4-chlorobenzylidene)amino]guanidine — hydrochloride.
Čisti robenidin: 1,3-bis[4-klorobenziliden)amino] gvanidin hidroklorid
Robenidine stock standard solution: 300 μg/ml
Osnovna standardna raztopina robenidina: 300 μg/ml
Weigh to the nearest 0,1 mg, 30 mg of robenidine standard substance (3.9).
30 mg standardnega robenidina (3.9) se natehta na 0,1 mg natančno.
Dissolve in acidified methanol (3.2) in a 100 ml graduated flask, make up to the mark with the same solvent and mix.
Raztopi se v nakisanem metanolu (3.2) v 100-mililitrski merilni bučki, dopolni se z istim topilom do oznake in premeša.
Wrap the flask with aluminium foil and store in a dark place.
Bučka se ovije v aluminijasto folijo in hrani v temi.
Robenidine intermediate standard solution: 12 μg/ml
Vmesna standardna raztopina robenidina: 12 μg/ml
Transfer 10,0 ml of the stock standard solution (3.9.1) into a 250 ml graduated flask, make up to the mark with the mobile phase (3.8) and mix.
10,0 ml osnovne standardne raztopine robenidina (3.9.1) se prenese v 250-mililitrsko merilno bučko, dopolni se z mobilno fazo (3.8) do oznake in premeša.
Into a series of 50 ml calibrated flasks, transfer 5,0, 10,0, 15,0, 20,0 and 25,0 ml of the intermediate standard solution (3.9.2).
V serijo 50-mililitrskih merilnih bučk se prenese 5,0, 10,0, 15,0, 20,0 in 25,0 ml vmesne standardne raztopine (3.9.2).
Make up to the mark with mobile phase (3.8) and mix.
Dopolni se z mobilno fazo (3.8) do oznake in premeša.
These solutions correspond to 1,2, 2,4, 3,6, 4,8 and 6,0 μg/ml of robenidine respectively.
Te raztopine ustrezajo koncentracijam robenidina 1,2, 2,4, 3,6, 4,8 in 6,0 μg/ml.
Water equivalent to HPLC grade.
Voda za HPLC
Glass column.
Steklena kolona
Constructed of amber glass fitted with a stopcock and a reservoir of approximately 150 ml capacity, internal diameter 10 to 15 mm, length 250 mm.
Iz temnega stekla, s petelinčkom in rezervoarjem z volumnom približno 150 ml, notranjega premera 10–15 mm, dolžine 250 mm
HPLC equipment with variable wavelength ultraviolet detector or diode array detector operating in the range of 250 to 400 nm.
Oprema za HPLC z ultravijoličnim detektorjem ali detektorjem s serijo diod, z nastavljivo valovno dolžino v območju 250–400 nm.
Liquid chromatographic column: 300 mm x 4 mm, C18 10 μm packing or equivalent.
Kolona za tekočinsko kromatografijo: 300 mm × 4 mm, C18, polnitev 10 μm ali enakovredna
Glass fibre filter paper (Whatman GF/A or equivalent).
Filtrski papir iz steklenih vlaken (Whatman GF/A ali enakovreden)
Membrane filters, 0,22 μm.
Membranski filtri, 0,22 μm
Membrane filters, 0,45 μm.
Membranski filtri, 0,45 μm
Robenidine is light-sensitive.
Robenidin je občutljiv na svetlobo.
Amber glassware shall be used in all operations.
Pri vseh postopkih se uporablja temna steklovina.
A blank feed shall be analysed to check that neither robenidine nor interfering substances are present.
Z analizo slepe krme se zagotovi, da niso prisotni niti robenidin niti moteče snovi.
A recovery test shall be carried out by analysing the blank feed (5.1.1) which has been fortified by addition of a quantity of robenidine, similar to that present in the sample.
Preskus izkoristka se izvede z analizo slepe krme (5.1.1), ki se ji doda količina amproliuma, podobna količini v vzorcu.
To fortify at a level of 60 mg/kg, transfer 3,0 ml of the stock standard solution (3.9.1) to a 250 ml conical flask.
Za koncentracijo 60 mg/kg se 3,0 ml osnovne standardne raztopine (3.9.1) prenese v 250-mililitrsko erlenmajerico.
Evaporate the solution to ca. 0,5 ml in a stream of nitrogen.
Raztopina se upari v toku dušika do približno 0,5 ml.
Add 15 g of the blank feed, mix and wait for 10 minutes before proceeding with the extraction step (5.2).
Doda se 15 g slepe krme, premeša, pusti 10 minut in nadaljuje z ekstrakcijo (5.2).
For the purpose of this method, the blank feed shall be similar in type to that of the sample and on analysis robenidine shall not be detected.
Pri tej metodi je vrsta slepe krme podobna vrsti vzorca in pri analizi se dokaže odsotnost robenidina.
Weigh to the nearest 0,01 g, approximately 15 g of the prepared sample.
Približno 15 g vzorca se natehta na 0,01 g natančno.
Transfer to a 250 ml conical flask and add 100,0 ml of acidified methanol (3.2), stopper and shake for one hour on the shaker (4.2).
Prenese se v 250-mililitrsko erlenmajerico, doda se 100,0 ml nakisanega metanola (3.2), zamaši se in stresa eno uro v stresalniku (4.2).
Filter the solution through a glass fibre filter paper (4.5) and collect the whole filtrate in a 150 ml conical flask.
Raztopina se filtrira skozi filtrirni papir iz steklenih vlaken (4.5) v 150-mililitrsko erlenmajerico.
Retain this solution for the purification step (5.3).
Ta raztopina se shrani za fazo čiščenja (5.3).
Purification
Čiščenje
Preparation of the aluminium-oxide column
Priprava kolone z aluminijevim oksidom
Insert a small glass-wool plug into the lower end of a glass column (4.1) and tamp it down using a glass rod.
V spodnji del steklene kolone se vstavi majhen zamašek iz steklene volne (4.1), ki se potlači s stekleno palčko.
Weigh out 11,0 g of the prepared aluminium oxide (3.5) and transfer to the column.
11,0 g pripravljenega aluminijevega oksida (3.5) se natehta in prenese v kolono.
Care shall be taken to minimise the exposure to the atmosphere during this stage.
Pazi se, da je pri tem postopku izpostavljenost zraku čim manjša.
Gently tap the loaded column at its lower end to settle the aluminium oxide.
Rahlo se udarja po spodnjem delu polne kolone, da se aluminijev oksid sesede.
Sample purification
Čiščenje vzorca
Transfer onto the column by pipette 5,0 ml of the sample extract prepared in (5.2) Rest the pipette tip close to the column wall and allow the solution to be absorbed onto the aluminium oxide.
Na kolono se s pipeto prenese 5,0 ml ekstrakta vzorca, pripravljenega v (5.2). Pipeta se nasloni na steno kolone, nato pa se pusti, da se raztopina absorbira na aluminijev oksid.
Elute the robenidine from the column using 100 ml methanol (3.1), at a flow rate of 2 to 3 ml/minute and collect the eluate in a 250 ml round bottomed flask.
Robenidin se eluira iz kolone s 100 ml metanola (3.1) s hitrostjo pretoka 2–3 ml/min, eluat pa se zbere v 250-mililitrsko bučko z okroglim dnom.
Evaporate the methanol solution to dryness under reduced pressure at 40 oC by means of a rotary film evaporator (4.3).
Raztopina metanola se upari do suhega pri znižanem tlaku in pri 40 oC v rotacijskem uparjalniku (4.3).
Re-dissolve the residue in 3 to 4 ml of mobile phase (3.8) and transfer quantitatively to a 10 ml graduated flask.
Ostanek se raztopi v 3–4 ml mobilne faze (3.8) in prenese v 10-mililitrsko merilno bučko.
Rinse the flask with several 1 to 2 ml portions of mobile phase and transfer these rinsings to the graduated flask.
Bučka se nekajkrat spere z 1–2 ml mobilne faze, izpirki pa se prenesejo v merilno bučko.
Make up to the mark with the same solvent and mix.
Dopolni se do oznake z istim topilom in premeša.
An aliquot is filtered through a 0,45 μm membrane filter (4.7).
Alikvot se prefiltrira skozi membranski filter 0,45 μm (4.7).
Reserve this solution for HPLC determination (5.4).
Ta raztopina se shrani za določanje s HPLC (5.4).
The following conditions are offered for guidance, other conditions may be used provided they yield equivalent results:
Naslednji pogoji se lahko uporabljajo kot smernice, lahko pa se uporabljajo drugi pogoji, če zagotavljajo enakovredne rezultate:
Liquid chromatographic column (4.4.1),
kolona za tekočinsko kromatografijo (4.4.1),
HPLC mobile phase (3.8),
mobilna faza HPLC (3.8),
Flow rate: 1,5 to 2 ml/minute,
hitrost pretoka: 1,5–2 ml/min,
Detector wavelength: 317 nm,
valovna dolžina detekcije: 317 nm,
Injection volume: 20 to 50 μl.
volumen, ki se vbrizga: 20–50 μl.
Check the stability of the chromatographic system, injecting the calibration solution (3.9.3) containing 3,6 μg/ml several times, until constant peak heights and retention times are achieved.
Stabilnost kromatografskega sistema se preveri z večkratnim vbrizgavanjem raztopine za umerjanje (3.9.3) s koncentracijo 3,6 μg/ml, dokler se ne dosežejo konstantne višine vrhov in konstantni retencijski časi.
Inject each calibration solution (3.9.3) several times and measure the peak heights (areas) for each concentration.
Vsaka raztopina za umerjanje (3.9.3) se večkrat vbrizga, za vsako koncentracijo pa se izmerijo višine (površine) vrhov.
Plot a calibration curve using the mean peak heights or areas of the calibration solutions as the ordinates and corresponding concentrations in μg per ml as abscissae.
Umeritvena krivulja se pripravi tako, da se na ordinato nanesejo srednje vrednosti višin ali površin vrhov raztopin za umerjanje, na absciso pa ustrezne koncentracije v μg/ml.
Inject the sample extract (5.3.2) several times, using the same volume as taken for the calibration solutions and determine the mean peak height (area) of the robenidine peaks.
Večkrat se vbrizga ekstrakt vzorca (5.3.2) z enakimi volumni, kakor se uporabljajo pri raztopini za umerjanje, nato pa se določijo srednje vrednosti višin (površin) vrhov robenidina.
From the mean height (area) of the robenidine peaks of the sample solution determine the concentration of the sample solution in μg/ml by reference to the calibration graph (5.4.2).
Koncentracija raztopine vzorca v μg/ml se določi iz srednje vrednosti višin (površin) vrhov robenidina iz umeritvene krivulje (5.4.2).
The content of robenidine w (mg/kg) in the sample is given by the following formula:
Vsebnost robenidina (w) (mg/kg) v vzorcu se izračuna po naslednji formuli:
c robenidine concentration of the sample solution in μg/ml,
c koncentracija robenidina v raztopini vzorca v μg/ml;
The identity of the analyte can be confirmed by co-chromatography, or by using a diode-array detector by which the spectra of the sample extract and the calibration solution (3.9.3) containing 6 μg/ml are compared.
Identiteta analita se lahko potrdi z dodatno kromatografijo ali z detektorjem s serijo diod, s katerim se primerjata spekter ekstrakta vzorca in spekter raztopine za umerjanje (3.9.3) s koncentracijo 6,0 μg/ml.
A sample extract is fortified by addition of an appropriate amount of calibration solution (3.9.3).
Ekstraktu vzorca se doda primerna količina raztopine za umerjanje (3.9.3).
The amount of added robenidine must be similar to the estimated amount of robenidine found in the sample extract.
Količina dodanega robenidina mora biti podobna ocenjeni količini robenidina v ekstraktu vzorca.
Only the height of the robenidine peak shall be enhanced after taking into account both the amount added and the dilution of the extract.
Povišan je le vrh robenidina ob upoštevanju dodane količine in razredčitve ekstrakta.
The peak width, at half of its maximum height, must be within approximately 10 % of the original width.
Širina vrha na polovici njegove največje višine mora biti v mejah približno 10 % prvotne širine.
For diode-array detection, this is typically within approximately 2 nm;
Za detekcijo s serijo diod je to ponavadi v območju približno 2 nm;
between 250 and 400 nm, the sample and standard spectra recorded at the peak apex on the chromatogram, must not be different for those parts of the spectrum within the range 10 % to 100 % of relative absorbance.
med 250 in 400 nm se spekter vzorca in spekter standarda na najvišji točki kromatografskega vrha za navedene dele spektra ne smeta razlikovati znotraj območja 10–100 % relativne absorbance.
between 250 and 400 nm, the spectra of the upslope, apex and downslope of the peak produced by the sample extract must not be different from each other for those parts of the spectrum within the range 10 % to 100 % of relative absorbance.
med 250 in 400 nm se spektri naraščanja, najvišje točke vrha in padanja vrha, pridobljeni iz ekstrakta vzorca, za navedene dele spektra ne smejo razlikovati znotraj območja 10–100 % relativne absorbance.
The difference between the results of two parallel determinations carried out on the same sample must not exceed 10 % of the higher result for robenidine content higher than 15 mg/kg.
Razlika med rezultatoma dveh vzporednih določanj, izvedenih na istem vzorcu, ne sme presegati 10 % višjega rezultata za vsebnost robenidina nad 15 mg/kg.
For a fortified blank sample the recovery shall be at least 85 %.
Za slepi vzorec z dodatkom je izkoristek najmanj 85 %.
An EC collaborative study was arranged in which four samples of poultry and rabbit feed, in meal or pelleted form were analysed by 12 laboratories.
ES je organizirala medlaboratorijsko študijo, pri kateri je 12 laboratorijev analiziralo štiri vzorce perutninske in kunčje krme v prahu in briketih.
Duplicate analyses were performed on each sample.
Vsak vzorec je bil analiziran dvakrat.
The results are given in the table below:
Rezultati so zbrani v spodnji preglednici:
Poultry
Perutninska krma
Rabbit
Kunčja krma
Meal
v prahu
Pellet
v briketih
Recovery [%]
Izkoristek [ %]
standard deviation of repeatability,
standardni odmik ponovljivosti;
standard deviation of reproducibility,
standardni odmik obnovljivosti;
coefficient of variation of reproducibility. %
koeficient variacije obnovljivosti v %.
DETERMINATION OF DICLAZURIL
DOLOČANJE DIKLAZURILA
(+)-4-chlorphenyl [2,6-dichloro-4-(2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazin-2-yl)phenyl] acetonitrile
(+)-4-klorfenil [2,6-dikloro-4-(2,3,4,5-tetrahidro-3,5-diokso-1,2,4-triazin-2-il) fenil] acetonitril
The method makes it possible to determine the level of diclazuril in feed and premixtures.
Ta metoda omogoča določanje ravni diklazurila v krmi in premiksih.
The limit of detection is 0,1 mg/kg, the limit of quantification is 0,5 mg/kg.
Meja določanja je 0,1 mg/kg, meja kvantifikacije pa 0,5 mg/kg.
After addition of an internal standard, the sample is extracted with acidified methanol.
Po dodatku notranjega standarda se vzorec ekstrahira z nakisanim metanolom.
For feed, an aliquot of the extract is purified on a C18 solid phase extraction cartridge.
Pri krmi se alikvot ekstrakta prečisti na kartuši C18 za ekstrakcijo v trdni fazi.
Diclazuril is eluted from the cartridge with a mixture of acidified methanol and water.
Diklazuril se eluira iz kartuše z mešanico nakisanega metanola in vode.
After evaporation, the residue is dissolved in DMF/water.
Po uparevanju se ostanek raztopi v raztopini DMF in vode.
For premixtures, the extract is evaporated and the residue is dissolved in DMF/water.
Pri premiksih se ekstrakt upari in nato se ostanek raztopi v raztopini DMF in vode.
The content of diclazuril is determined by ternary gradient reversed-phase high-performance liquid chromatography (HPLC) using a UV detector.
Vsebnost diklazurila se določi s tekočinsko kromatografijo visoke ločljivosti (HPLC) z reverzno fazo s ternarnim gradientom, z uporabo UV-detektorja.
Water, equivalent to HPLC-grade
Voda, za HPLC
Tetrabutylammonium hydrogen sulphate (TBHS)
Tetrabutilamonijev hidrogen sulfat (TBHS)
Acetonitrile, equivalent to HPLC grade
Acetonitril, za HPLC
Methanol, equivalent to HPLC grade
Metanol, za HPLC
N, N-dimethylformamide (DMF)
N, N-dimetilformamid (DMF)
Hydrochloric acid, ρ20 = 1,19 g/ml
Klorovodikova kislina, ρ20 = 1,19 g/ml
Standard substance: diclazuril II-24: (+)-4-chlorphenyl [2,6-dichloro-4-(2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazin-2-yl) phenyl] acetonitrile with guaranteed purity, E771
Standardna snov: diklazuril II-24: (+)-4-klorfenil [2,6-diklor-4-(2,3,4,5-tetrahidro-3,5-diokso-1,2,4-triazin-2-il) fenil] acetonitril, zajamčene čistosti, E771.
Diclazuril stock standard solution, 500 μg/ml
Osnovna standardna raztopina diklazurila, 500 μg/ml
Weigh to the nearest 0,1 mg, 25 mg of diclazuril standard substance (3.8) in a 50 ml graduated flask.
25 mg standardne snovi diklazurila (3.8) se natehta na 0,1 mg natančno in prenese v 50-mililitrsko merilno bučko.
Dissolve in DMF (3.6), make up to the mark with DMF (3.6) and mix.
Raztopi se v DMF (3.6), bučka se dopolni z DMF (3.6) do oznake in premeša.
Wrap the flask with aluminium foil or use amber flask and store in the refrigerator.
Bučka se ovije v aluminijasto folijo ali pa se uporabi rjava bučka ter shrani v hladilniku.
At a temperature of ≤ 4 oC the solution is stable for 1 month.
Pri temperaturi ≤ 4 oC je raztopina stabilna 1 mesec.
Diclazuril standard solution, 50 μg/ml
Standardna raztopina diklazurila, 50 μg/ml
Transfer 5,00 ml of the stock standard solution (3.8.1) into a 50 ml graduated flask, make up to the mark with DMF (3.6) and mix.
5,00 ml osnovne standardne raztopine (3.8.1) se prenese v 50-mililitrsko merilno bučko, dopolni se z DMF (3.6) do oznake in premeša.
Internal standard substance: 2,6 dichloro-α-(4-chlorophenyl)-4-(4,5 dihydro-3,5-dioxo-1,2,4-triazine-2 (3H) — yl) α-methylbenzene-acetonitrile
Snov, ki je notranji standard: 2,6 dikloro-α-(4-klorofenil)-4-(4,5 dihidro-3,5-diokso-1,2,4-triazin-2 (3H) – il) α-metilbenzen-acetonitril.
Internal stock standard solution, 500 μg/ml
Osnovna raztopina notranjega standarda, 500 μg/ml
Weigh to the nearest 0,1 mg 25 mg of internal standard substance (3.9) in a 50 ml graduated flask.
25 mg notranjega standarda (3.9) se natehta na 0,1 mg natančno in prenese v 50-mililitrsko merilno bučko.
Internal standard solution, 50 μg/ml
Raztopina notranjega standarda, 50 μg/ml
Transfer 5,00 ml of the internal stock standard solution (3.9.1) into a 50 ml graduated flask, make up to the mark with DMF (3.6) and mix.
5,00 ml osnovne raztopine notranjega standarda (3.9.1) se prenese v 50-mililitrsko merilno bučko, dopolni se z DMF (3.6) do oznake in premeša.
Internal standard solution for premixtures, p/1000 mg/ml
Raztopina notranjega standarda za premikse, p/1000 mg/ml
(p = nominal content of diclazuril in the premixture in mg/kg)
(p = nominalna vsebnost diklazurila v mg/kg v premiksu)
Weigh to the nearest 0,1 mg p/10 mg of the internal standard substance in a 100 ml graduated flask, dissolve in DMF (3.6) in a ultrasonic bath (4.6), make up to the mark with DMF and mix.
p/10 mg notranjega standarda se natehta na 0,1 mg natančno in prenese v 100-mililitrsko merilno bučko, raztopi se v DMF (3.6) v ultrazvočni kopeli (4.6), dopolni se z DMF do oznake in premeša.
Wrap the flask with aluminium foil or use amber flask and store in a refrigerator.
Bučka se ovije v aluminijasto folijo ali pa se uporabi rjava bučka ter shrani v hladilniku.
Calibration solution, 2 μg/ml.
Raztopina za umerjanje, 2 μg/ml
Pipet 2,00 ml diclazuril standard solution (3.8.2) and 2,00 ml internal standard solution (3.9.2) into a 50 ml graduated flask.
2,00 ml standardne raztopine diklazurila (3.8.2) in 2,00 ml raztopine notranjega standarda (3.9.2) se odpipetira v 50-mililitrsko merilno bučko.
Add 16 ml DMF (3.6), make up to the mark with water and mix.
Doda se 16 ml DMF (3.6), bučka se dopolni z vodo do oznake in premeša.
solid phase extraction cartridge, e.g. Bond Elut, size: 1 cc, sorbent weight: 100 mg.
Ekstrakcijska kartuša za trdno fazo C18, npr. Bond Elut, velikost: 1 cc, masa absorbenta: 100 mg
Extraction solvent: acidified methanol.
Ekstrakcijsko topilo: nakisani metanol
Pipet 5,0 ml hydrochloric acid (3.7) into 1000 ml of methanol (3.5), and mix.
5,0 ml klorovodikove kisline (3.7) se odpipetira v 1000 ml metanola (3.5) in premeša.
Mobile phase for HPLC
Mobilna faza za HPLC
Eluent A: ammonium acetate — tetrabutylammonium hydrogen sulphate solution.
Eluent A: raztopina amonijevega acetata in tetrabutilamonijevega hidrogen sulfata
Dissolve 5 g ammonium acetate (3.2) and 3,4 g TBHS (3.3) in 1000 ml water (3.1) and mix.
5 g amonijevega acetata (3.2) in 3,4 g TBHS (3.3) se raztopi v 1000 ml vode (3.1) ter premeša.
Eluent B: acetonitrile (3.4).
Eluent B: acetonitril (3.4)
Eluent C: methanol (3.5).
Eluent C: metanol (3.5)
Equipment for ternary gradient HPLC
Oprema za HPLC s terciarnim gradientom
Liquid chromatographic column, Hypersil ODS, 3 μm packing, 100 mm x 4,6 mm, or equivalent
Kolona za tekočinsko kromatografsko kolono, Hypersil ODS, polnitev 3 μm, 100 mm x 4,6 mm ali enakovredna
UV detector with variable wavelength adjustment or diode array detector
UV-detektor z nastavljivo valovno dolžino ali detektor s serijo diod.
Membrane filter, 0,45 μm
Membranski filter, 0,45 μm
Vacuum manifold
Vakuumski ventil
Blank feed
Slepa krma
A blank feed shall be analysed to check that neither diclazuril nor interfering substances are present.
Z analizo slepe krme se zagotovi, da niso prisotni niti diklazuril niti moteče snovi.
The blank feed shall be similar in type to that of the sample and on analysis diclazuril or interfering substances shall not be detected.
Vrsta slepe krme je podobna vrsti vzorca in z analizo se dokaže odsotnost diklazurila ali motečih substanc.
Recovery test
Preskus izkoristka
A recovery test shall be carried out by analysing the blank feed which has been fortified by addition of a quantity of diclazuril similar to that present in the sample.
Preskus izkoristka se izvede tako, da se analizira slepa krma, ki se ji doda toliko diklazurila, kolikor ga je v vzorcu.