CS228259B1 - Method for determining lobeline chloride content in countersmoking chewing-gums - Google Patents
Method for determining lobeline chloride content in countersmoking chewing-gums Download PDFInfo
- Publication number
- CS228259B1 CS228259B1 CS697381A CS697381A CS228259B1 CS 228259 B1 CS228259 B1 CS 228259B1 CS 697381 A CS697381 A CS 697381A CS 697381 A CS697381 A CS 697381A CS 228259 B1 CS228259 B1 CS 228259B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- lobelin
- chloride
- chewing
- gums
- chewing gum
- Prior art date
Links
- MXYUKLILVYORSK-HBMCJLEFSA-N (-)-lobeline Chemical compound C1([C@@H](O)C[C@H]2N([C@H](CCC2)CC(=O)C=2C=CC=CC=2)C)=CC=CC=C1 MXYUKLILVYORSK-HBMCJLEFSA-N 0.000 title claims description 32
- MXYUKLILVYORSK-UHFFFAOYSA-N (+/-)-allo-lobeline Natural products C1CCC(CC(=O)C=2C=CC=CC=2)N(C)C1CC(O)C1=CC=CC=C1 MXYUKLILVYORSK-UHFFFAOYSA-N 0.000 title claims description 31
- 235000015218 chewing gum Nutrition 0.000 title claims description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims description 22
- 238000000034 method Methods 0.000 title claims description 10
- 229930013610 lobeline Natural products 0.000 title description 2
- 229960002339 lobeline Drugs 0.000 title description 2
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 claims description 26
- 229940112822 chewing gum Drugs 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004811 liquid chromatography Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims 3
- 230000005526 G1 to G0 transition Effects 0.000 claims 1
- 230000002738 anti-smoking effect Effects 0.000 description 10
- 238000011088 calibration curve Methods 0.000 description 8
- 238000010828 elution Methods 0.000 description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 230000010354 integration Effects 0.000 description 4
- 230000000391 smoking effect Effects 0.000 description 4
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Chemical compound OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 238000003556 assay Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229930013930 alkaloid Natural products 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000013375 chromatographic separation Methods 0.000 description 2
- 238000009223 counseling Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000002552 dosage form Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 2
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 2
- 229960002715 nicotine Drugs 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000005586 smoking cessation Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000600 sorbitol Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 208000011580 syndromic disease Diseases 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- HORQAOAYAYGIBM-UHFFFAOYSA-N 2,4-dinitrophenylhydrazine Chemical compound NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HORQAOAYAYGIBM-UHFFFAOYSA-N 0.000 description 1
- GRZMOSSVIPFGFF-GNJLJDPWSA-N 2-[(2r,6s)-6-[(2s)-2-hydroxy-2-phenylethyl]-1-methylpiperidin-2-yl]-1-phenylethanone;sulfuric acid Chemical compound OS(O)(=O)=O.C1([C@@H](O)C[C@H]2N([C@H](CCC2)CC(=O)C=2C=CC=CC=2)C)=CC=CC=C1.C1([C@@H](O)C[C@H]2N([C@H](CCC2)CC(=O)C=2C=CC=CC=2)C)=CC=CC=C1 GRZMOSSVIPFGFF-GNJLJDPWSA-N 0.000 description 1
- -1 3-orbitol Substances 0.000 description 1
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 208000002193 Pain Diseases 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000001919 adrenal effect Effects 0.000 description 1
- 230000002716 ataractic effect Effects 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 150000003943 catecholamines Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001055 chewing effect Effects 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000007884 disintegrant Substances 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000008101 lactose Substances 0.000 description 1
- 239000007937 lozenge Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 210000001034 respiratory center Anatomy 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 235000019615 sensations Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007909 solid dosage form Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 230000035900 sweating Effects 0.000 description 1
- 239000003826 tablet Substances 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Confectionery (AREA)
- Medicinal Preparation (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Description
Vynález oa týká spósobu stánovenia chloridu lobelínia v protifajčiarokych žuvačkách.The invention relates to a method for determining lobelin chloride in anti-smoking chewing gum.
Protifajčiarske liečebné metody sa opierajú o psychoterapeutické pÓ3obenie, ktoré sa často doplňuje přidáváním ataraktík, alebo aplikáciou látok, ktoré v opojení o fajčením vyvolávajú nepříjemné chuťové a čuchové pocity a tým navodzujú odpor k fajčeniu. Na tento ciel’ oa užívajú v poolednej době přípravky o obsahom soli lobelínia, ako látky na odvykanie od fajčenia., alebo na znechutenie fajčenia. Táto látka javí podobné farmakologické účinky ako nikotin. Oba alkaloidy otimulujú dychové centrum. Sú totiž schopné povzbudit po injekčnom podávaní uvďnenie oerotonínu. Typická pre oba alkaloidy je ich vlastnost uvolňovat z nadobličkovej drene katecholaminy· Jeho póoobením sa vyvolá tzv. Joot-Jochimov lobelín - nikotinový syndrom Joot J., Jochim K.: Med. Kliň. 54, 1049, 1959. Tento syndrom spočívá v tom, že pri fajčení po predchádsajúeom perorálnom podávaní lobelínu vznikajú nepříjemné vedl’sjšie pocity, ako závrate, bolesti hlavy, dráždenie na vracanie, silné potenie a bolesti v oblasti ordca, čiže tento reflex ovplyvňuje odpor k fajčeniu a prispieva k odvykaniu od fajčenia. Lobelín oa podává perorálne vo formě soli a to ako síran, alebo hydrochlorid lobelínia. Aplikuje oa v pevných liekových formách a to vo formě tabletiek, paotiliek a vo formě žuvačiek.Anti-smoking therapies rely on psychotherapeutic efficacy, often supplemented by the addition of ataractics, or by the application of substances that, in smoking, induce unpleasant taste and olfactory sensations and thereby induce resistance to smoking. For this purpose, they are using pooled salt products containing lobelin as a smoking cessation agent or a smoking cessation agent. This substance has similar pharmacological effects to nicotine. Both alkaloids stimulate the respiratory center. They are able to stimulate the release of oerotonin after injection. Typical of both alkaloids is their ability to release catecholamines from adrenal pulp. Joot-Jochim's Lobelin - Nicotine Syndrome Joot J., Jochim K .: Med. Kline. 54, 1049 (1959). This syndrome consists in the fact that smoking after previous oral administration of lobelin gives rise to unpleasant side effects such as dizziness, headache, vomiting irritation, severe sweating and pain in the ordca area, which affects resistance and contributes to quitting smoking. Lobelin oa is administered orally in the form of a salt, such as lobelin sulphate or hydrochloride. It is applied oa in solid dosage forms in the form of tablets, palatines and chewing gum.
Zloženie všetkých troch typov liekových foriem oa líši navzájom iba použitými pomocnými látkami a spósobom ich galenického opracovania.The composition of all three types of dosage forms differs from each other only by the auxiliaries used and the manner of their galenic processing.
Prvú odbornú správu o výrobě lobelínu za účelom jeho použitia ako zložky protifajčiarokych prípravkov vypracoval Urban J.í Lobelin.Študijná správa O.S.VTEI farm.prum.č.175, 1962.The first expert report on the manufacture of lobelin for its use as an anti-smoking ingredient was prepared by Urban J. Lobelin. Study report O.S.VTEI farm.prum.
Analytickému ohodnoteniu chloridu lobelínia oa věnovali viacerí autoři. Jeho atanovenie v žuvačkách naráželo na značná taž- 5 228 2S9 kosti pre termolabilitu lobelínu, ktorá komplikuje jeho extrakciu zo žuvačky. VzhTadom k tomu, že chlorid lobelínia patří medzi separanda, nie j:e možné používat, protifajčiaroke žuvačky bezjpresného určenia jeho koncentrácie v tejto liekovej formě.Several authors gave analytical evaluation of lobelin chloride o and o. Its chewing in chewing gums encountered considerable tensile bones for lobelin thermolability, which complicated its extraction from the chewing gum. Defining as the fact that one of the lobeline chloride separanda not j: E may be used, protifajčiaroke gum bezjpresného determining the concentration of the dosage form.
Polarografické otanovenie chloridu lobelínia navrhované Šautavým, Šantavý F.: Čeo.čeo.lek.56, 1, 1943 a Šantavý F.: Čes. čeo.lek.57, 109, 1944 sa·nemohlo realizovat pře už uvedená náročná extrakciu zo žuvačiek a termolabilitu lobelínu. Kvantitativné oddelenie chloridu lobelínia od ootatných sáčiaotok Žuvačky sa nedalo previest’ bez toho, že by nenastal jeho rozklad a preto aj výsledky polarografického stanovenia boli nereprodukovateTné.Polarographic determination of lobelin chloride proposed by Šautavý, Šantavý F .: Čeo.čeo.lek.56, 1, 1943 and Šantavý F .: Čes. 57, 109, 1944 could not be accomplished with the aforementioned demanding chewing gum extraction and lobelin thermolability. The quantitative separation of lobelin chloride from the ottotic bags of Chewing gum could not be transferred without decomposition and therefore the results of the polarographic assay were not reproducible.
Fotometrická metodu, ktorá sa používá na stanovenie chloridu lobelínia po jeho převedení na acetofenon na základe farebnej reakcie o 2,4-dinitrofenyIhydrazinom popíoaná Marternom K., Schillom C.: Svenok.farmac.Tidskr.54, 461, 1950 nebolo možné použit pre intenzívně zafarbenie, vzniklé vplyvom reakcie žuvačkovej hmoty s týmto reagentom, čiže ani tento postup nebol vhodný na sledovaný áčel.The photometric method used to determine lobelin chloride after its conversion to acetophenone based on the 2,4-dinitrophenylhydrazine color reaction described by Martern K., Schill C .: Svenok.farmac.Tidskr.54, 461, 1950 could not be used intensively the coloring resulting from the reaction of the chewing gum mass with this reagent, so this procedure was not suitable for the eye of interest.
Na základe uvedeného sa javilo potřebné vypracovat taká metodu, ktorá by umožnila reprodukovateTné otanovenie chloridu lobelínia v protifajčiarokych žuvačkách, čo doslal’ nebolo možné, lým sa aj negativné ovplyvnila možnost jeho využívania v protifajčiarskych poradniach. Žuvačky, ktoré sa používájá na tento áčel, obsahujá okrem soli lobelínia ako pomocné látky 3orbitol, propylénglykol, žuvačkovú hmotu a ako chutové korigeno cukor, alebo mliečny cukor. Pri vypracovaní analytického postupu sa sledoval cieT dospiet k metóde, ktorá by dávala exaktně a reprodukovateTné výsledky stanovenia·On the basis of the above, it appeared necessary to develop a method which would allow reproducible determination of lobelin chloride in anti-smoking chewing gums, which was not possible and would also negatively affect its use in anti-smoking counseling. The chewing gum used for this sack contains, besides lobelin salt, as adjuvants, 3-orbitol, propylene glycol, chewing gum mass and as a taste corrected sugar or milk sugar. In developing the analytical procedure, the objective was to arrive at a method that would give exact and reproducible assay results.
Vypracoval sa spósob stanovenia chloridu lobelínia v protifajčiarokych žuvačkách na bázi jeho prevedenia na acetofenon ca zictěný acetofenon izoluje destiléciou a stanoví sa pri teplote 20 °C a tlaku 12,7 MPa kvapalinovou chromatografiou, pričom sa ako stacionárna fáza použije silikagél o chemicky naviazaným oktadecyloilanom o velkosti zrniek 10 jum a ako rozpušfadlová oáotava metanol □ vodou, v pomere 1í2.A method for the determination of lobelin chloride in anti-smoking chewing gum based on its conversion to acetophenone was prepared and the acetophenone was isolated by distillation and determined by liquid chromatography at 20 ° C and 12 MPa using a chemically bound octadecyloilane-size silica gel 10 µm grains and as a solvent solvent methanol-water, at a ratio of 1 2.
Žuvačky určené k príprave kalibračnej křivky sa převedu na acetofenon obdobné ako sa to robí v žuvačkách, v ktorých saChewing gums intended to prepare the calibration curve are converted to acetophenone similar to that of chewing gums in which
- 4 228 2S9 má kbejjji 3 táno vit a po izolácii yzniklého acetofenonu sa tento stanoví kvapalinovou chromatografiou. Výsledky stanovenia v uvedenom koncentračnom rozsahu sú reprodukovatelná, čo umožnilo analýzu protifajčiarskych žuvačiek a tým aj ich přípravu, a bezpečné používanie v protifajčiarskych poradniach, čo predtým nebolo možné.The 4,228 2S9 has a thaw of 3 and after isolation of the acetophenone formed, this is determined by liquid chromatography. The results of the assay in this concentration range are reproducible, allowing analysis of the anti-smoking chewing gums and hence their preparation, and safe use in anti-smoking counseling centers, which was previously not possible.
Tabulkatable
Experimentálně výsledky r« výpočet pre zostrojenie kalibračnej křivky /x/ 'Experimental results r «calculation for construction of calibration curve / x / '
/x/ Odhad omerodajnej odchylky regreonej priamky o = 546 KorelaČný koeficient rVY = 0,994/ x / Estimation of the standard error of the regression line o = 546 Correlation coefficient r VY = 0,994
Lineárnou regresiou sa z nameraných hodnot vypočítala nižšie uvedená rovnica kalibračnej křivky.The calibration curve equation below was calculated from the measured values by linear regression.
y = 1077 + 186611 x, kde hodnota y je plocha ohromatografického píku v integračných jednotkách, hodnota x je udávané množstvo chloridu lobelínia v 100 g žuvačky. Výsledky sú zhrnuté v tabulke.y = 1077 + 186611 x, where y is the area of the chromatographic peak in integration units, x is the reported amount of lobelin chloride in 100 g of chewing gum. The results are summarized in the table.
Na obr. 1 je kalibračná křivka na stanovenie chloridu lobelínia.In FIG. 1 is a calibration curve for the determination of lobelin chloride.
Na obr. 2 je chromatogram žuvačky o obsahom chloridu lobelínia s chuťovým korigentom oo sacharózou a so sorbitolom.In FIG. 2 is a chromatogram of a gum of lobelinium chloride with a taste coefficient for sucrose and sorbitol.
Na obr. 3 je chromatogram žuvačky s obsahom chloridu lobelínia s chuťovými korigentami o laktozou a oo sorbitolom. , j t In FIG. 3 is a chromatogram of a chewing gum containing lobelin chloride with flavoring lozenges and sorbitol. , jt
ΑλΛτ- t /e eAx«iue/ear«(M funtffcy «.fc/aiezv eá/.r/efa /dwAiykΑλΛτ- t / e eAx "iue / ear" (M funtffcy ".fc / aiezv eá / .r / efa / dwAiyk"
Na obr. 1 na ose x sa uvádza hmotnost chloridu lobelínia v 100 g žuvačky. Na ose y je znázorněná plocha křivky v integračných jednotkách. čiara 1 představuje závislost’ plochy chromátografickej vlny od koncentrácie chloridu lobelínia v žuvačke, pričom sa plocha udává v integračných jednotkách. Udaná hodnota je priemer zo šieotich meraní. Čiara 2 znázorňuje regresnú křivku vypočítanáIn FIG. 1 on the x-axis shows the weight of lobelin chloride in 100 g of chewing gum. The y-axis shows the area of the curve in integration units. line 1 represents the dependence of the area of the chromatographic wave on the concentration of lobelin chloride in the chewing gum, the area being given in integration units. The value given is the average of the six measurements. Line 2 shows the regression curve calculated
- 5 lineárnou regreoiou zo všetkých meraní. 23i 258- 5 linear regression from all measurements. 23i 258
Na obr. 2 elučná vlna 3 je chromatografickou vlnou acetofenonu. Elučné vlny 4 a 5 sú chromátografickými vlnami zložiek rozpíájfadlovej síotavy.In FIG. 2 elution wave 3 is acetophenone chromatographic wave. Elution waves 4 and 5 are the chromatographic waves of the components of the disintegrant mesh.
Na obr. 3 je chromatogram žuvačky a obsahom chloridu lobelínia s chuťovými korigentami laktózou a aorbitolom. Elučné vlna 3 je elučnou vlnou acetofenonu. Vlny 4 a 5 sú elučnými vlnami zložiek rozpíáťadlových odstav.In FIG. 3 is a chromatogram of chewing gum containing lobelin chloride with flavoring agents lactose and aorbitol. Elution wave 3 is an acetophenone elution wave. The waves 4 and 5 are the elution waves of the components of the weaning components.
Na obr. 4 je chromatogram o obsahom chloridu lobelínia s chuťovým korigentom a oacharózou. Elučná vlna 3 je vlna acetofenonu, vlny 4 a 5 sú elučné vlny zložiek rozpúšťadiel.In FIG. 4 is a chromatogram containing lobelin chloride containing flavor and oacharose. Elution wave 3 is acetophenone wave, waves 4 and 5 are elution waves of solvent components.
Příprava kalibračnej křivkyPreparation of the calibration curve
Pracovalo oa o nasledujúcimi přesnými koncentráciami chloridu lobelínia v protifajčiarakych žuvačkách a to : 0,03, 0,045, 0,060, 0,075, 0,09 na 100 g žuvačky. Žuvačky oa jemne posekají a navážia sa preone do Erlenmayerovej banky oo zábruoom a zábruoovou zátkou. Přidá sa 20 ml 95% liehu, 10 ml 1 mol hydroxidu draselného a 10 ml deotilovanej vody. Zmes oa vaří 4 hodiny pod opátným chladičom. Potom oa přidá 100 ml deotilovanej vody a po výměně spatného chladiča za zostupný sa pokračuje v deotilácii. Destilát sa zachycuje do 100 ml odmernej banky preone do 100 ml.The following exact concentrations of lobelin chloride in anti-smoking chewing gums were used: 0.03, 0.045, 0.060, 0.075, 0.09 per 100 g of chewing gum. The chewing gums gently and gently weigh and are weighed preone into an Erlenmayer flask with a baffle and baffle plug. 20 ml of 95% alcohol, 10 ml of 1 mol of potassium hydroxide and 10 ml of deotified water are added. The mixture was boiled under reflux for 4 hours. Subsequently, 100 ml of deionized water are added and deodorization is continued after replacement of the bad condenser with the descending condenser. Collect the distillate in a 100 ml volumetric flask up to 100 ml.
Z tohoto roztoku oa odpipetuje 10 pl a nanáša oa na kolonu kvapalinového chromatografu. Ghromatografické delenie a 3tanovenie acetofenónu, ktorý sa připravil z lobelínu oa robí následujícím opooobom. Použije oa kvapalinový chromatograf o detektorom o premenlivou vlnovou dížkou. Plocha píkov oa hodnotí integrátorom. Použije oa kolona o rozměrochCpx25 cm. Náplň kolony ailikagél o chemicky viazaným oktadecylsilanom o velkosti zrniek 10 jam. Ako rozpíšťadlová oístava je vhodná oístava : metanol - voda 1 : 2. Pracuje sa při teplote 20 °C o 12,7 MPa. Nanáša oa 10 pl vzorky Hamiltonovou mikropipetou. Rýchlooť prietoku elučnej odstavy, ktorá je vhodná pře tito aaaalýzu je 1,2 ml/min. Detekcia oa robí v UV ovetle pri 249 nm.From this solution, α is pipetted 10 µl and loaded α on a liquid chromatograph column. The chromatographic separation and determination of acetophenone, which was prepared from lobelin o and makes the following opooob. Uses oa liquid chromatograph with variable wavelength detector. The area of the peaks about and evaluated by the integrator. It will use a x25x25 cm column. 10 µm bead packed with chemically coupled octadecylsilane and a silica gel column. The solvent is: methanol - water 1: 2. Working at 20 ° C at 12.7 MPa. Dispense about 10 µl of samples with a Hamilton micropipette. The elution weaning flow rate suitable for this and analysis is 1.2 ml / min. Detection of α and δ is done in UV light at 249 nm.
Kecíže nebolo možné zootrojiť kalibrační křivku z hodnot získaných po převedení chloridu lobelínia na acetofenon preWhile it was not possible to cut the calibration curve from the values obtained after converting lobelin chloride to acetophenone for
228 259 .>traty po extrakcii zo žuvačiek, idealizovalo oa vyhodnotenie výsledkov analýz z kalibračnej křivky, zootrojenej už uvedeným )ooobom#228 259.> Lines after extraction from chewing gum, idealized by and evaluating the results of the analysis from the calibration curve, cut to the above) ooob #
Stanovenie chloridu lobelínia v protifajčiarokych žuvačkách g žuvačky jemne pooekanej oa naváži preone do Erlenmayerovej banky oo zábruoom a oo zábruoovou zátkou. Přidá oa 20 ml liehu, 10 ml roztoku hydroxidu draselného o koncentrácii 1 mol/l a 10 ml deotilovanej vody. Zmes oa vaří 4 hodiny pod opátným chladičom. Potom oa přidá 100 ml deotilovanej vody a po výměně spatného chladiča na zootupný sa pokračuje v destilácii. Destilát oa zachycuje do 100 ml odmernej banky, přesné sa doplní po značku. Z toho roztoku oa odpipetuje 10 jol a nanááa oa na kolonu.· Chromatografické delenie a otanovenie acetofenonu, ktorý sa připravil z lobelínu, oa previedlo už popíoaným opóoobom v příklade 1,metodou kvapalinovej chromatografie.Determination of lobelin chloride in anti-smoking chewing gums g of finely-oat chewing gum and weighing preone into an Erlenmayer flask with a stopper and a stopper. Add about 20 ml of alcohol, 10 ml of 1 M potassium hydroxide solution and 10 ml of de-water. The mixture was boiled under reflux for 4 hours. Then, 100 ml of deionized water are added and distillation is continued after the replacement of the bad condenser to a zootic. Collect the distillate oa in a 100 ml graduated flask, make up to the mark with precision. From this solution oa is pipetted 10 µl and applied oa onto the column · Chromatographic separation and determination of acetophenone prepared from lobelin, and carried out by the previously described method in Example 1, by liquid chromatography method.
Vyhodnotenie výoledkov získaných kvapalinovou chromatografiou oa robí z kalibračnej křivky.The evaluation of the liquid chromatograms obtained from a day makes a calibration curve.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS697381A CS228259B1 (en) | 1981-09-22 | 1981-09-22 | Method for determining lobeline chloride content in countersmoking chewing-gums |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS697381A CS228259B1 (en) | 1981-09-22 | 1981-09-22 | Method for determining lobeline chloride content in countersmoking chewing-gums |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS228259B1 true CS228259B1 (en) | 1984-05-14 |
Family
ID=5417991
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS697381A CS228259B1 (en) | 1981-09-22 | 1981-09-22 | Method for determining lobeline chloride content in countersmoking chewing-gums |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS228259B1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117723680A (en) * | 2024-02-08 | 2024-03-19 | 苏州博研医药科技有限公司 | Separation detection method for lobelia hydrochloride impurity |
-
1981
- 1981-09-22 CS CS697381A patent/CS228259B1/en unknown
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117723680A (en) * | 2024-02-08 | 2024-03-19 | 苏州博研医药科技有限公司 | Separation detection method for lobelia hydrochloride impurity |
| CN117723680B (en) * | 2024-02-08 | 2024-05-03 | 苏州博研医药科技有限公司 | Separation detection method for lobelia hydrochloride impurity |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Siridevi et al. | RP-HPLC method for quantification of Empagliflozin in pharmaceutical formulation | |
| Ding et al. | Determination of deltamethrin and its metabolite 3-phenoxybenzoic acid in male rat plasma by high-performance liquid chromatography | |
| Makhani et al. | Development and validation of vierordt's spectrophotometric method for simultaneous estimation of Drotaverine and Nimesulide combination | |
| Minase et al. | Development and validation of analytical method for simultaneous estimation of cilnidipine and olmesartan medoxomil in bulk and tablet dosage form by HPTLC | |
| de Córdova et al. | Sensitive and selective determination of diclofenac sodium in pharmaceutical preparations by solid phase ultraviolet absorptiometry | |
| Bhanu et al. | RP-HPLC method for quantification of bilastine and monteleukast sodium in pharmaceutical dosage form | |
| CS228259B1 (en) | Method for determining lobeline chloride content in countersmoking chewing-gums | |
| Lott et al. | The determination of paraquat | |
| Honma et al. | Neurotoxicity and metabolism of methyl bromide in rats | |
| Braimah et al. | Impurity profiling of paracetamol dosage forms used in maiduguri metropolis | |
| Malgundkar et al. | Validated HPTLC method for simultaneous determination of metformin hydrochloride and glibenclamide in combined dosage form | |
| Watson et al. | Assay for trimethoprim in serum and urine by means of ion-pair chromatography. | |
| Shaikh et al. | Development and validation of stability indicating RP-HPLC and UV method for simultaneous quantitation of repaglinide and sitagliptin phosphate in combination | |
| Krishna et al. | Method development and validation of RP-HPLC method for the determination of sumatriptan in bulk and pharmaceutical dosage form | |
| Stanley et al. | Gas-chromatographic method for residues of Baygon and metabolites in plant tissues | |
| Madhusudhan et al. | A RP-HPLC method development and validation for simultaneous estimation of metformin HCl and rosiglitazone in bulk and tablet dosage form | |
| Mathur et al. | Novel Method Development, Validation and Stability Indicating Assay Method for Rivastigmine Tartarate Capsule by HPLC | |
| Muthyala et al. | Stability indicating RP-HPLC method development and validation for the quantitative estimation chlorthalidone in API and tablet dosage form | |
| Barsuhn | The measurement of nanogram amounts of piperidine in tissues by gas chromatography | |
| Kumar et al. | RP-HPLC and UV method development for simultaneous estimation of doxofylline, montelukast and levocetirizine dihydrochloride in pharmaceutical dosages form | |
| Gupta et al. | Simultaneous reverse phase-high performance liquid chromatography (RP-HPLC) estimation of azelastine hydrochloride, fluticasone propionate, and phenyl ethyl alcohol in dymista (MEDA) nasal spray | |
| Ritter | Thin-layer densitometric determination of muzolimine (BAY g 2821), a structurally new diuretic drug, at the nanogram level in biological fluids | |
| RU2824822C1 (en) | Method for oral delivery of chemical compounds into fish of genus nothobranchius for preclinical studies | |
| Kurtz et al. | Gas chromatographic determination of total active ingredient content of Karathane Technical and Karathane WD. I. Development of the method | |
| Sakano et al. | Simultaneous Determination of Acetaminophen, Caffeine and Dihydrocodeine Phosphate in Tablets by High Performance Liquid Chromatography |