CN103592347A - Novel quick detecting method for dioxopromethazine hydrochloride - Google Patents
Novel quick detecting method for dioxopromethazine hydrochloride Download PDFInfo
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- CN103592347A CN103592347A CN201310578870.2A CN201310578870A CN103592347A CN 103592347 A CN103592347 A CN 103592347A CN 201310578870 A CN201310578870 A CN 201310578870A CN 103592347 A CN103592347 A CN 103592347A
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- dioxopromethazine hydrochloride
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Abstract
The invention provides a novel method for measuring the content of dioxopromethazine hydrochloride by adopting an ion selective electrode method. Compared with the traditional method, the novel method has the advantages of simple experimental instrument, low testing cost, simplicity, quickness, relatively accurate measuring result, relatively wide linear range and relatively high sensitivity, and is a simplest feasible analysis method for measuring the content of the dioxopromethazine hydrochloride.
Description
Technical field
The invention belongs to the technical field of Pharmaceutical Analysis, be specifically related to the potentiometric analysis method of dioxopromethazine hydrochloride quantitative test, especially the assay method of active constituent content in dioxopromethazine hydrochloride medicine.
Background technology
Ion-selective electrode is that a kind of optional membrane of utilization produces selective response to measure or to indicate the electrode of effects of ion activity to specific ion.The principle of work of ion selective electrode method is as follows: indicator electrode (also claims working electrode, the present invention uses chlorion to select electrode) electrical potential energy indicate the variation of tested ion activity (or concentration), the current potential of contrast electrode (the present invention uses the full mercurous chloride electrode that closes) is not subject to test solution to form the impact changing, there is more constant numerical value, by indicator electrode and contrast electrode, jointly immerse while forming primary element in test solution and measure the electromotive force obtaining, according to nernst equation, can obtain tested ion activity (or concentration).The method instrument and equipment is inexpensive, light, it is simple and easy, quick, reliable to operate, the range of linearity is wide, selectivity and highly sensitive (detection limit 10
-5mg/ml), can directly measure liquor sample, the color of solution and turbidity generally do not affect the result of test, are simple and easy, the most feasible a kind of new methods of measuring dioxopromethazine hydrochloride.
Dioxopromethazine hydrochloride (C
17h
20n
2o
2sHCl) chemistry 10-(2-dimethylamino-isopropyl) by name phenothiazine-5, the hydrochloride of 5-dioxide, this medicine has stronger antitussive effect, and has antihistamine, releasing smooth muscle spasm, anti-inflammatory drawn game anaesthetic effect, without the toxicity of the internal organs such as liver kidney.After antitussive effect comes across and takes medicine 30 ~ 60 minutes, continue 4 ~ 6 hours or longer.Be applicable to antibechic, relieving asthma, be also applicable to treat nettle rash and cutaneous pruritus etc.Common bad reaction is sleepy, weak etc.Work high above the ground and steering vehicle, the person's of operating machine forbidding.Therapeutic dose and dosis toxica approach, and must not surpass maximum dose.Therefore the promethazine hydrochloride active constituent content in tablet being monitored, is the needs that ensure health.
At present, the method for measuring dioxopromethazine hydrochloride amount mainly be take high performance liquid chromatography and ultraviolet spectrophotometry as main, but these methods need sample to carry out complicated processing before mensuration, and the range of linearity is not wide, also very high to the requirement of sample preparation.In addition, expensive, the complicated operation of these instruments and Pharmaceutical Analysis process have secondary environmental pollution, analysis cost high.
Summary of the invention
The present invention aims to provide a kind of new method of simple, Accurate Determining dioxopromethazine hydrochloride content.
Summary of the invention comprises: proving installation, test electrode, test condition, total ionic strength adjustment buffer degree regulator solution and quantitative analysis method.
1) proving installation
The present invention adopts PHS-2C type acidometer directly to read potential value (above blastoid magnetic instrument plant), adopting DF-101D heat collecting type constant-temperature heating magnetic stirring apparatus (Gongyi City Yu Hua Instrument Ltd.) is test condition control device, measures dioxopromethazine hydrochloride content in unlimited glass container.Fig. 1 is the connection diagram of medicine dioxopromethazine hydrochloride determinator.
2) test electrode
This invention take pCL-1Q9 type chlorion select electrode (Shanghai Russell science and technology company limited) for working electrode, 217 type saturated calomel electrodes be the content of reference electrode (going up blastoid magnetic instrument plant) testing drug dioxopromethazine hydrochloride.
3) test condition
This invents described condition determination: stir speed (S.S.) 2000rpm/min, mixing time are 7min, pH5～6, and 25 ℃ of temperature, buffer solvent is that total ionic strength adjustment buffer degree regulates buffer solution.The present invention is preferred for measuring the dioxopromethazine hydrochloride content in dioxopromethazine hydrochloride medicine.
4) total ionic strength adjustment buffer degree regulator solution
The total ionic strength adjustment buffer that this invention is used is that concentration is 0.01mol/L, the CH that pH value is
3cOOH-CH
3cOONa buffer solution.
5) quantitative analysis method
This invention be take calibration curve method as the main method of quantitative test medicine dioxopromethazine hydrochloride active constituent content.
Accompanying drawing explanation
Fig. 1 medicine dioxopromethazine hydrochloride determinator schematic diagram.
Wherein, V is voltage table, and C is that indicator electrode (chlorion selection electrode), R are that contrast electrode (the full mercurous chloride electrode that closes), L are that solution to be measured, B are that beaker, M are magnetic force heating stirrer.
Embodiment
Below in conjunction with embodiment, describe the present invention in detail, but the following examples are only preferably implemented for the present invention
Mode, protection scope of the present invention is not limited to this, any be familiar with those skilled in the art this
In the technical scope that invention discloses, according to technical scheme of the present invention and inventive concept thereof, be equal to replacement or changed, within all should being encompassed in protection scope of the present invention.
Total ionic strength adjustment buffer degree regulates the preparation of buffer solution: in 1000ml beaker, add 500ml deionized water, 25ml glacial acetic acid, 58g sodium chloride and 12g sodium citrate, be stirred to completely and dissolve.Beaker is placed in cooling bath, slowly adds NaOH solution (6mol/L) and carefully stir evenly, with PHS-2C type precision acidity meter (Shanghai Lei Ci instrument plant), test, making pH is 5.Be cooled to room temperature, proceed in 1000ml volumetric flask, with deionized water, be diluted to graticule, fully shake up.
The foundation of dioxopromethazine hydrochloride typical curve: with AL204 type electronic balance (Shanghai plum Teller —Tuo benefit Instrument Ltd.) take respectively 5,0.5,0.05,0.005,0.0005mg promethazine hydrochloride standard items (Di Kang pharmaceutcal corporation, Ltd provides), proceed to respectively in 5 50ml volumetric flasks, with deionized water, be diluted to graticule, shaking up and obtaining concentration is 1 * 10
-1, 1 * 10
-2, 1 * 10
-3, 1 * 10
-4, 1 * 10
-5the dioxopromethazine hydrochloride standard solution of mg/ml.By shown in accompanying drawing 1, assemble after experimental provision, first 50ml deionized water is added in beaker, add 2 buffer solution, open magnetic force heating stirrer switch, at 25 ℃ of stir speed (S.S.) 2000 rpm/min, temperature, after cleaning electrode is stable to current potential, read blank electromotive force.Get volumetric flask No. 1, all proceed in clean and dry 50ml beaker, add 2 buffer solution (final pH=5～6 of gained solution), at 25 ℃ of stir speed (S.S.) 2000 rpm/min, temperature, stir 7min, stop 1min, read and record equilibrium potential value.Then use the same method, measure respectively the equilibrium potential value of test solution in 2,3,4, No. 5 volumetric flasks.Measurement result be take the negative logarithm of dioxopromethazine hydrochloride concentration (mg/ml) as horizontal ordinate, equilibrium potential reading (mV) are as ordinate carries out linear regression, obtains typical curve equation: y=-20.200x-36.343(R
2=0.9065).
The mensuration of dioxopromethazine hydrochloride tablet content: promethazine hydrochloride tablet (the 25mg/ sheet of getting 10 different batches (5 slices/batch), Taiyuan, Shanxi pharmaceutcal corporation, Ltd) grind respectively, take the abrasive material that weight is 0.5000g, in 20ml deionized water, with very opening up the ultrasonic 20min of QT2060 Ultrasound Instrument (Tianjin Rui Pu Electronic Instrument, Limited), filter, again by residue in 20ml deionized water, with after the ultrasonic 15min of Ultrasound Instrument, filtrate is mixed with the ultrasonic filtrate obtaining for the first time, surely be dissolved in 250ml volumetric flask, more ultrasonic 10min, it is fully dissolved.Then when setting up with typical curve, under identical experiment condition, measure, by the above-mentioned typical curve equation of equilibrium potential value substitution reading, calculate the content of dioxopromethazine hydrochloride in tablet, result is as shown in table 1.
Table 1 medicine dioxopromethazine hydrochloride assay result
In addition, the mensuration comparing result of the present invention and other classic methods is as shown in table 2.
Table 2 distinct methods is measured the contrast of dioxopromethazine hydrochloride result
| Detection method | Concentration sensing range (mg/ml) | Minimum detectability (mg/ml) | The recovery (%) | Relative standard deviation (RSD, %) |
| The present invention | 1.0×10 -5～1.0×10 -1 | 10 -5 | 98.50 | 0.9 |
| Ultraviolet spectrophotometry 1 | 0.20～0.50 | 0.20 | 102.68 | 1.2 |
| High performance liquid chromatography 1 | 0.02～0.30 | 0.02 | 101.80 | 0.6 |
| Ultraviolet spectrophotometry 2 | 0.20～0.50 | 0.20 | 99.05 | 1.1 |
| High performance liquid chromatography 2 | 0.10～0.30 | 0.10 | 100.56 | 0.6 |
The above results shows, compare with classic method, not only experimental apparatus is simple in the present invention, testing cost is low, and easy, quick, measurement result relatively accurately, the range of linearity is wider, sensitivity is higher, is simple and easy, the most feasible a kind of analytical approach of measuring dioxopromethazine hydrochloride.
Claims (3)
1. a new method of measuring dioxopromethazine hydrochloride content, is characterized in that, adopting chlorion to select electrode is that working electrode, saturated calomel electrode are reference electrode, and application potentiometry is measured the content of dioxopromethazine hydrochloride effective ingredient.
2. method according to claim 1, is characterized in that, described condition determination is: stir speed (S.S.) 2000rpm/min, mixing time are 5 min, and 25 ℃ of temperature, with CH
3cOOH-CH
3cOONa is that total ionic strength adjustment buffer degree regulates buffer solution, and its pH scope is 5～6.
3. method according to claim 1 and 2, is characterized in that, described method is carried out quantitative test with employing calibration curve method to sample, and for measuring the content of the dioxopromethazine hydrochloride effective constituent of dioxopromethazine hydrochloride medicine.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105606739A (en) * | 2016-02-25 | 2016-05-25 | 山东省食品药品检验研究院 | Q-Orbitrap high-resolution mass spectrum method for identifying illegal addition of dioxopromethazine in Chinese patent medicine without reference substance |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090130087A1 (en) * | 2006-04-05 | 2009-05-21 | Charles Lee | Method for measuring the content of a botulinum toxin in a formulation |
| CN201653968U (en) * | 2010-05-19 | 2010-11-24 | 辽宁省建设科学研究院 | Detector of ion content in concrete |
| CN102914573A (en) * | 2012-10-24 | 2013-02-06 | 大连大学 | Method for measuring content of diphenhydramine hydrochloride |
-
2013
- 2013-11-17 CN CN201310578870.2A patent/CN103592347A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090130087A1 (en) * | 2006-04-05 | 2009-05-21 | Charles Lee | Method for measuring the content of a botulinum toxin in a formulation |
| CN201653968U (en) * | 2010-05-19 | 2010-11-24 | 辽宁省建设科学研究院 | Detector of ion content in concrete |
| CN102914573A (en) * | 2012-10-24 | 2013-02-06 | 大连大学 | Method for measuring content of diphenhydramine hydrochloride |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105606739A (en) * | 2016-02-25 | 2016-05-25 | 山东省食品药品检验研究院 | Q-Orbitrap high-resolution mass spectrum method for identifying illegal addition of dioxopromethazine in Chinese patent medicine without reference substance |
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Application publication date: 20140219 |