CS262055B1 - Process for qualitative analysis of residual nicotinonitrile together with nicotinonide in products of nicotinonitrile hydrolysis - Google Patents
Process for qualitative analysis of residual nicotinonitrile together with nicotinonide in products of nicotinonitrile hydrolysis Download PDFInfo
- Publication number
- CS262055B1 CS262055B1 CS872433A CS243387A CS262055B1 CS 262055 B1 CS262055 B1 CS 262055B1 CS 872433 A CS872433 A CS 872433A CS 243387 A CS243387 A CS 243387A CS 262055 B1 CS262055 B1 CS 262055B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- nicotinonitrile
- residual
- hydrolysis
- products
- nicotinonide
- Prior art date
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- GZPHSAQLYPIAIN-UHFFFAOYSA-N 3-pyridinecarbonitrile Chemical compound N#CC1=CC=CN=C1 GZPHSAQLYPIAIN-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title claims description 7
- 230000007062 hydrolysis Effects 0.000 title claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 title claims description 3
- 238000004451 qualitative analysis Methods 0.000 title 1
- DFPAKSUCGFBDDF-UHFFFAOYSA-N nicotinic acid amide Natural products NC(=O)C1=CC=CN=C1 DFPAKSUCGFBDDF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000005152 nicotinamide Nutrition 0.000 claims abstract description 6
- 239000011570 nicotinamide Substances 0.000 claims abstract description 6
- 229960003966 nicotinamide Drugs 0.000 claims abstract description 6
- 238000003965 capillary gas chromatography Methods 0.000 claims abstract description 4
- 238000004445 quantitative analysis Methods 0.000 claims abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 229920000151 polyglycol Polymers 0.000 claims description 2
- 239000010695 polyglycol Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- -1 nicotinamide amine Chemical class 0.000 abstract 1
- 238000004458 analytical method Methods 0.000 description 8
- KXDAEFPNCMNJSK-UHFFFAOYSA-N Benzamide Chemical compound NC(=O)C1=CC=CC=C1 KXDAEFPNCMNJSK-UHFFFAOYSA-N 0.000 description 4
- 239000000523 sample Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000005526 G1 to G0 transition Effects 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- CCDWGDHTPAJHOA-UHFFFAOYSA-N benzylsilicon Chemical compound [Si]CC1=CC=CC=C1 CCDWGDHTPAJHOA-UHFFFAOYSA-N 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000010813 internal standard method Methods 0.000 description 2
- 238000004255 ion exchange chromatography Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229920001921 poly-methyl-phenyl-siloxane Polymers 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 1
- DFPAKSUCGFBDDF-ZQBYOMGUSA-N [14c]-nicotinamide Chemical compound N[14C](=O)C1=CC=CN=C1 DFPAKSUCGFBDDF-ZQBYOMGUSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000001886 ciliary effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000000887 hydrating effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229960003512 nicotinic acid Drugs 0.000 description 1
- 235000001968 nicotinic acid Nutrition 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000006884 silylation reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004809 thin layer chromatography Methods 0.000 description 1
- 235000019156 vitamin B Nutrition 0.000 description 1
- 239000011720 vitamin B Substances 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
Souběžná kvantitativní analýza zbytkového nikotinonitrilu společně s nikotinamiděin metodou kapilární plynové chromatograťíe s přímým dávkováními na kolonu.Parallel residual quantitative analysis nicotinonitrile together with nicotinamide amine by capillary gas chromatography with direct column dosing.
Description
Hydratací nikotinonitrilu za bazické katalýzy a při vhodné teplotě lze připravit nikotinamid, biologicky účinnou formu jednoho z vitaminů B (niacin).By hydrating nicotinonitrile under basic catalysis and at a suitable temperature, nicotinamide, the biologically active form of one of the vitamins B (niacin), can be prepared.
Většina dosud publikovaných metod analýzy nikotinamidu a nikotinonitrilu jsou metody chromatografieiké, jako je chromatografie na tenké vrstvě, ionexová chromatografie, vysoce účinná kapalinová chromatografie a plynová chromatografie na náplňové i kapilární koloně. V řadě případů se jedná o metody analýzy časově náročné, ať už díky složitější předúpravě vzorků (například silylace při analýze plynovou chromatografií), či zdlouhavosti saihotné analýzy, nebo jsou analýzy málo citlivé pro nízké koncentrace zbytkového nikotinonitrilu (například vysolovací vysoce účinná kapilární chromatografie).Most of the published methods of nicotinamide and nicotinonitrile analysis are chromatography methods such as thin layer chromatography, ion exchange chromatography, high performance liquid chromatography and gas chromatography on both packed and capillary columns. In many cases, these are time-consuming analysis methods, either due to more complex sample pretreatment (for example, silylation in gas chromatography analysis) or the lengthyness of the self-analysis, or the analyzes are less sensitive to low residual nicotinonitrile concentrations (for example salting-out high performance capillary chromatography).
Nyní bylo nalezeno, že analýzu zbytkového nikotinamidu v produktech hydrolýzy nikotinonitrilu metodou kapilární plynové chromatografie je možno provádět tak, že se roztok produktu v organickém rozpouštědle, například methanolu nebo ethanolu, dávkuje na začátek skleněné nebo křemenné kapilární kolony smočené stacionární fází typu silikonu, například fenylmethylsilikonovým olejem nebo polyglykolu při teplotě 60 °C až teplota varu rozpouštědla metodou přímého dávkování na kolonu.It has now been found that capillary gas chromatography analysis of residual nicotinamide in nicotinonitrile hydrolysis products can be carried out by feeding a solution of the product in an organic solvent such as methanol or ethanol to a glass or quartz capillary column wetted with a stationary silicone-type phase such as phenylmethylsilicone. oil or polyglycol at a temperature of 60 ° C to the boiling point of the solvent by the direct-dosing method on the column.
Roztok vzorku s přiváženým standardem se dávkuje speciální stříkačkou s dlouhou jehlou až na začátek kolony smočěné silikonovou stacionární fází, chromatografuje se při programové teplotě kolony, separované složky se detekuji plamenoionizačním detektorem, odezvy detektoru jsou korigovány kalibračními faktory, které se předem zjistí analýzou směsi o známém složení navážené ze standardních látek. Výpočet se provede metodou vnitřního standardu.The sample solution with the fed standard is dosed with a special syringe with a long needle up to the beginning of the column wetted with a silicone stationary phase, chromatographed at the column temperature, separated components are detected by a flame ionization detector, detector responses are corrected by calibration factors. composition weighed from standard substances. The calculation is performed using the internal standard method.
Kvantitativní výsledky metody jsou srovnatelné s výsledky z vysoce účinné kapalinové chromatografie, jak bylo ověřeno. Analýza kapilární plynovou chromatografií podle vynálezu je rychlá, nevyžaduje speciální úpravu vzorku a umožňuje stanovit i malé koncentrace zbytkového nikotinonitrilu společně s nikotinamidem.The quantitative results of the method are comparable to those from high performance liquid chromatography, as verified. The capillary gas chromatography analysis of the present invention is rapid, does not require special sample treatment, and allows small concentrations of residual nicotinonitrile to be determined together with nicotinamide.
Způsob analýzy podle vynálezu ilustruje níže uvedený příklad.The analysis method according to the invention is illustrated by the example below.
Příklad provedeníExemplary embodiment
1 vzorku se odváží do 10 ml odměrky a její obsah se doplní metanolem či etanoIem po» rysku. 1 ml tohoto roztoku se odpipetuje do další odměrky (10 ml), smísí se s 1 ml metanolického (nebo etanolického) roztoku vnitřního standardu (tj. 2,01 mg benzamidu). Tento roztok se dávkuje injekční stříkačkou typu Hamilton s dlouhou ocelovou jehlou až na začátek křemenné klapilární kolony udržované při teplotě 600 Celsia. Použije-li se kapilární kolona z taveného velmi čistého» kysličníku křemičitého o délce 25 m a vnitřním průměru 0,32 milimetru, smočená stacionární fází např. fenylmetylsilikonovým olejem. Kolona je umístěna v termostatu plynového» chromatogramu, vybaveným zařízením pro dávkování přímo na kolonu, plamenoionizačním detektorem »a vyhodnocovacím Nařízením. Termostat chromatografu se rychle ihned po nástřiku ohřeje z 60 °C na počátečních 100 ° Celsia a pak jeho teplota stoupá rychlostí 5 °C/min a oid 3. minuty rychlostí 10 °C/min do 200 °C, kde se udrží ještě asi 3 minuty. Nosný plyn dusík či hélium protéká rychlostí 3 ml/min. Složky jsou eluovány v pořadí: nikotinonitril, benzamid, nikotinamid. Odezvy jednotlivých složek se korigují faktory, získanými vyhodnocením analýzy roztoku kalibrační směsi navážené z čistých standardů a vypočte se procentuální zastoupení jednotlivých složek při použití metody vnitřního standardu.Weigh 1 sample into a 10 ml measuring cup and make up to the mark with methanol or ethanol. Pipette 1 ml of this solution into another measuring cup (10 ml) and mix with 1 ml of methanolic (or ethanolic) internal standard solution (ie 2,01 mg of benzamide). This solution is dosed with a Hamilton steel syringe with a long steel needle up to the beginning of a quartz ciliary column maintained at 60 ° C. If a capillary column of fused, very pure silica of 25 m long and 0.32 mm internal diameter is used, it is wetted with a stationary phase, for example with phenylmethyl silicone oil. The column is placed in a gas »chromatogram thermostat equipped with a device for dosing directly to the column, a flame ionization detector» and an evaluation regulation. The thermostat of the chromatograph is heated immediately after injection from 60 ° C to the initial 100 ° C and then its temperature rises at 5 ° C / min and oid for 3 minutes at 10 ° C / min to 200 ° C, where it is kept for about 3 minutes. The carrier gas nitrogen or helium flows at a rate of 3 ml / min. The components are eluted in the order: nicotinonitrile, benzamide, nicotinamide. The responses of the individual components are corrected by the factors obtained from the analysis of the calibration standard solution weighed from the pure standards and the percentage of the individual components is calculated using the internal standard method.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS872433A CS262055B1 (en) | 1987-04-06 | 1987-04-06 | Process for qualitative analysis of residual nicotinonitrile together with nicotinonide in products of nicotinonitrile hydrolysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS872433A CS262055B1 (en) | 1987-04-06 | 1987-04-06 | Process for qualitative analysis of residual nicotinonitrile together with nicotinonide in products of nicotinonitrile hydrolysis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CS243387A1 CS243387A1 (en) | 1988-07-15 |
| CS262055B1 true CS262055B1 (en) | 1989-02-10 |
Family
ID=5361480
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS872433A CS262055B1 (en) | 1987-04-06 | 1987-04-06 | Process for qualitative analysis of residual nicotinonitrile together with nicotinonide in products of nicotinonitrile hydrolysis |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS262055B1 (en) |
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1987
- 1987-04-06 CS CS872433A patent/CS262055B1/en unknown
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| Publication number | Publication date |
|---|---|
| CS243387A1 (en) | 1988-07-15 |
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