SU1048382A1 - Qualidil qualitative determination method - Google Patents
Qualidil qualitative determination method Download PDFInfo
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- SU1048382A1 SU1048382A1 SU823461364A SU3461364A SU1048382A1 SU 1048382 A1 SU1048382 A1 SU 1048382A1 SU 823461364 A SU823461364 A SU 823461364A SU 3461364 A SU3461364 A SU 3461364A SU 1048382 A1 SU1048382 A1 SU 1048382A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- chloroform
- sample
- qualitative determination
- solution
- qualidil
- Prior art date
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- 238000000034 method Methods 0.000 title claims abstract description 16
- WOUMHLGSMDVJHS-UHFFFAOYSA-L 3-benzyl-1-[6-(3-benzyl-1-azoniabicyclo[2.2.2]octan-1-yl)hexyl]-1-azoniabicyclo[2.2.2]octane;dichloride Chemical compound [Cl-].[Cl-].C1CC(C(CC=2C=CC=CC=2)C2)CC[N+]12CCCCCC[N+](CC1)(C2)CCC1C2CC1=CC=CC=C1 WOUMHLGSMDVJHS-UHFFFAOYSA-L 0.000 title 1
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 230000035945 sensitivity Effects 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012491 analyte Substances 0.000 claims abstract description 5
- UDSAIICHUKSCKT-UHFFFAOYSA-N bromophenol blue Chemical compound C1=C(Br)C(O)=C(Br)C=C1C1(C=2C=C(Br)C(O)=C(Br)C=2)C2=CC=CC=C2S(=O)(=O)O1 UDSAIICHUKSCKT-UHFFFAOYSA-N 0.000 claims abstract description 4
- 150000001875 compounds Chemical class 0.000 claims abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract 2
- 239000000126 substance Substances 0.000 claims description 2
- 230000002934 lysing effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000012797 qualification Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- LOUPRKONTZGTKE-WZBLMQSHSA-N Quinine Chemical compound C([C@H]([C@H](C1)C=C)C2)C[N@@]1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OC)C=C21 LOUPRKONTZGTKE-WZBLMQSHSA-N 0.000 description 2
- LOUPRKONTZGTKE-UHFFFAOYSA-N cinchonine Natural products C1C(C(C2)C=C)CCN2C1C(O)C1=CC=NC2=CC=C(OC)C=C21 LOUPRKONTZGTKE-UHFFFAOYSA-N 0.000 description 2
- 150000007530 organic bases Chemical class 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- LOUPRKONTZGTKE-LHHVKLHASA-N quinidine Chemical compound C([C@H]([C@H](C1)C=C)C2)C[N@@]1[C@H]2[C@@H](O)C1=CC=NC2=CC=C(OC)C=C21 LOUPRKONTZGTKE-LHHVKLHASA-N 0.000 description 2
- DGPMCYQIJOUUFY-UHFFFAOYSA-N 1-azabicyclo[2.2.2]octan-3-yl benzoate;hydrochloride Chemical group Cl.C1N(CC2)CCC2C1OC(=O)C1=CC=CC=C1 DGPMCYQIJOUUFY-UHFFFAOYSA-N 0.000 description 1
- PKYZWCLYWCKYNX-UHFFFAOYSA-N 2,2,6,6-tetramethyl-1-azoniabicyclo[2.2.2]octane;bromide Chemical compound Br.C1CN2C(C)(C)CC1CC2(C)C PKYZWCLYWCKYNX-UHFFFAOYSA-N 0.000 description 1
- LHGMHYDJNXEEFG-UHFFFAOYSA-N 4-[4-(dimethylamino)phenyl]iminocyclohexa-2,5-dien-1-one Chemical compound C1=CC(N(C)C)=CC=C1N=C1C=CC(=O)C=C1 LHGMHYDJNXEEFG-UHFFFAOYSA-N 0.000 description 1
- 235000001258 Cinchona calisaya Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229960003216 aceclidine Drugs 0.000 description 1
- WRJPSSPFHGNBMG-UHFFFAOYSA-N acetic acid 1-azabicyclo[2.2.2]octan-3-yl ester Chemical compound C1CC2C(OC(=O)C)CN1CC2 WRJPSSPFHGNBMG-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940125782 compound 2 Drugs 0.000 description 1
- AFGPCIMUGMJQPD-UHFFFAOYSA-L disodium;4,5-dihydroxynaphthalene-2,7-disulfonate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)C1=CC(O)=C2C(O)=CC(S([O-])(=O)=O)=CC2=C1 AFGPCIMUGMJQPD-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- -1 imi n Chemical compound 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000003158 myorelaxant agent Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 230000003389 potentiating effect Effects 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- PZMAHNDJABQWGS-UHFFFAOYSA-N quifenadine Chemical compound C1N(CC2)CCC2C1C(O)(C=1C=CC=CC=1)C1=CC=CC=C1 PZMAHNDJABQWGS-UHFFFAOYSA-N 0.000 description 1
- 229960004466 quifenadine Drugs 0.000 description 1
- 229960001404 quinidine Drugs 0.000 description 1
- 229960000948 quinine Drugs 0.000 description 1
- SBYHFKPVCBCYGV-UHFFFAOYSA-N quinuclidine Chemical group C1CC2CCN1CC2 SBYHFKPVCBCYGV-UHFFFAOYSA-N 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Investigating Or Analysing Biological Materials (AREA)
Abstract
СПОСОБ. КАЧЕСТВЕННОГО ОПРЕДЕЛЕНИЯ КЙАЛИДИЛА с .использованием /обработки пробы анализируемого вещества реагентом с получением окрашенного соединени , о т л и ч а ю щ и йс тем, что, с целью повышени чувствительности способа, пробу ана- . лизируемого в ества последователь ио обрабатывают бромфеноловым синим :в щелочной среде, хлороформом, раствором сол ной кислоты с получением ркрашеиного сло хлороформа.METHOD QUALITATIVE DETERMINATION OF KYALIDIL using a sample / treatment of an analyte with a reagent to obtain a colored compound, that is, in order to increase the sensitivity of the method, the sample is ana-. lysing follower is treated with bromophenol blue: in an alkaline medium, chloroform, and a solution of hydrochloric acid to form a r-colored layer of chloroform.
Description
ОABOUT
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Изобретение относитс к способам качественного анализа фармацевтических препаратов и может быть использовано в услови х аптек, контрольноаналитических и заводских лабораторий , в судебно-химической экспертизеThe invention relates to methods for the qualitative analysis of pharmaceutical preparations and can be used in pharmacies, control analytical and factory laboratories, in the forensic chemical examination
Квалидил 1, б-бисг- (З -бензил-хинуклидил-l )-гексана дихлорид вл етс сильнодействующим мышечным релаксантом курареподобного действи .Qualidyl 1, b-bis-3 (3-benzyl-quinuclidyl-1) -hexane dichloride is a potent muscle relaxant with a curare-like effect.
Известен способ качественного определени квалидила путем обработки пробы анализируемого вещества динатриевой солью хромотроповой кислоты с образованием окрашенного соединени i .A known method for the qualitative determination of qualification by treating a sample of an analyte with chromotropic acid disodium salt to form colored compound i.
Недостатком этого способа вл етс относительно невысока чувствительность (80-100 мкг/мл).The disadvantage of this method is the relatively low sensitivity (80-100 µg / ml).
Наиболее близким к предлагаемому по технической сущности и достигаемым результатам вл етс способ опредени квалидила- путем обработки пробы анализируемого вещества раствором аммониевой соли кислоты Рейнеке с получением окраьаенного соединени 2 . . . The closest to the proposed technical essence and the achieved results is the method of determining qualification by treating a sample of the analyte with a solution of the ammonium salt of Reineke to obtain a colored compound 2. . .
Недостатком данного способа вл етс относительно невысока , чувстBHTejibHOCTb (80-10Q мкг/мл) .The disadvantage of this method is relatively low, feeling BHTejibHOCTb (80-10Q µg / ml).
Цель изобретени - повышение чувствительности способа.The purpose of the invention is to increase the sensitivity of the method.
Поставленна цель достигаетс тем, что согласно способу определени квалидила. пробу анализируемого вещества последовательно обрабатывают промфеноловым синим в щелочной среде, хлороформом, раствором сол ной кислоты с получением окрашенного сло хлороформа. The goal is achieved by the fact that according to the method of determining qualification. A sample of the analyte is sequentially treated with industrial phenol blue in an alkaline medium, chloroform, and hydrochloric acid solution to form a colored layer of chloroform.
Последовательное осуществление;описанных стадий составл ет отличительную особенность способа.The sequential implementation of the described stages constitutes a distinctive feature of the method.
Условием проведени реакции вл етс одновременное существование в ионизированной форме и красител и органического основани , что далеко не всегда возможно. Если же такой интервал Н существует, то он обьгано находитс в слабокислой или в близкой к нейтральной среде, где краситель находитс , э форме одногThe condition for the reaction is the simultaneous existence in ionized form of both the dye and the organic base, which is not always possible. If such an interval H exists, then it is bound to be in a weakly acidic or close to neutral medium, where the dye is, in the form of one
зар дного аниона, окрашенного в желтый цвет. Вследствие этого образующиес ионные ассоциаты также имеют одинаковую желтую окраску Сдюкс 400415нм ) в редких случа х малиновую С /лаке - 570-580 нм) , что в реакции с бромфенольным синим (БФ) нивелирует свойства органических оснований и не дает возможности их идентифицировать .charge anion colored yellow. As a result, the formed ionic associates also have the same yellow color (Sjux 400415nm) in rare cases (crimson C / lacquer - 570-580 nm), which in reaction with bromophenol blue (BF) levels the properties of organic bases and makes it impossible to identify them.
и м е р. В малеиновую пробирку с пришлифованной пробкой .внос т;,2-3 мГ препарата, 1 мл 0,1 М раствора NaOH, 4 капли (лО,2. мл) 0,04%ного раствора 6ФС и 1 мл хлороформа. 5 Содержимое пробирки встр хивают в течение 30 сек и наблюдают синее окрашивание хлороформного сло . Затем по капл м, встр хива пробирку после каждого добавлени , внос т 1 мл 0,1 М раствора ЙСб. При э5:ом хлороформ приобретает сначала зеленую, а затем желтую окраску. and me. In a maleic test tube with a ground up stopper., 2-3 mg of the preparation, 1 ml of 0.1 M NaOH solution, 4 drops (LO, 2 ml) of a 0.04% 6FS solution and 1 ml of chloroform. 5 The contents of the tube are shaken for 30 seconds and a blue color of the chloroform layer is observed. Then, drop by drop, after shaking the tube after each addition, add 1 ml of 0.1 M YSb solution. At e5: chloroform gets first green and then yellow.
При анализе квалидила в интьекционном растворе (2-5%) в пробирку достаточно внести 1-2 капли исследуемой жидкости и далее аналогично описанному , When analyzing the qualification in the injection solution (2-5%), it is enough to add 1-2 drops of the test liquid to the tube and then, similarly to that described,
Дл характеристики чувствительности реакции определён мол рный коэф0 фициент поглощени ассоциата по отношению к 0,0003 М раствору квалидила (fj iaKC- 5 14 X 10) . Исход из йакС Р;.ассчитаны коэффициенты чувствительности Седела Ng 0, 012 и коэф5 фициенты Коха и Коха-ДеДица Vx -0,6. Минимально открываема концентраци Смин 0.,75 мкг/мл. To characterize the sensitivity of the reaction, the molar absorption coefficient of the associate with respect to a 0.0003 M solution qualifier (fj iaKC- 5 14 X 10) was determined. The outcome of Sedela's sensitivity coefficients Ng 0, 012 and the coefficients of Koch and Koch-DeDitz Vx -0.6 are calculated from yakS P; The minimum openable concentration is Cmin 0., 75 µg / ml.
Аналогичной реакции не дает ни один препара группы хинуклидина (ацеклидин, оксилидин, темехин, имехи н , фенкарол, хинин, хинидин) , а также продукты их синтеза (3-оксихинуклидин , хинуклидон-3) .None of the quinuclidine group preparations (aceclidine, oxylidine, temechin, imi n, phencarol, quinine, quinidine), as well as the products of their synthesis (3-hydroxyinuclidine, quinuclidon-3), give a similar reaction.
Сравнение данных предлагаемого способа с описанными в нормативнотехнической документации представлены в таблице.Comparison of data of the proposed method with those described in the regulatory documentation presented in the table.
Предлагаемый способ позвол ет повысить чувствительность способа в 10 раз.The proposed method allows to increase the sensitivity of the method 10 times.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU823461364A SU1048382A1 (en) | 1982-06-24 | 1982-06-24 | Qualidil qualitative determination method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU823461364A SU1048382A1 (en) | 1982-06-24 | 1982-06-24 | Qualidil qualitative determination method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU1048382A1 true SU1048382A1 (en) | 1983-10-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU823461364A SU1048382A1 (en) | 1982-06-24 | 1982-06-24 | Qualidil qualitative determination method |
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| Country | Link |
|---|---|
| SU (1) | SU1048382A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999021854A1 (en) * | 1997-10-24 | 1999-05-06 | Newlaxant Llc | Bis-quaternary ammonium derivatives as neuromuscular relaxants |
-
1982
- 1982-06-24 SU SU823461364A patent/SU1048382A1/en active
Non-Patent Citations (1)
| Title |
|---|
| 1 ВФС 42-888-74. 2, ВФС 42-887-74 (прототип). ; * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999021854A1 (en) * | 1997-10-24 | 1999-05-06 | Newlaxant Llc | Bis-quaternary ammonium derivatives as neuromuscular relaxants |
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