Method for detecting related substances in Tolterodine tartrate raw material or preparation

A technology of tolterodine tartrate and related substances, which is applied in the field of detection of related substances of tolterodine tartrate raw materials or preparations, and can solve problems such as inappropriate purity of the main peak, inappropriate peak purity, and reduction of the organic phase ratio in the mobile phase , to achieve the effect of accurate and reliable results, simple operation and strong specificity

Inactive Publication Date: 2012-03-07
LUNAN PHARMA GROUP CORPORATION
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Under these conditions, the retention time of tolterodine tartrate is about 4.0min, and the DAD detector shows that the main peak peak purity is not suitable, then reduce the proportion of the organic phase in the mobile phase, the peak shape is poor, and the peak purity is still not suitable, and at the same time The test results show that the selected wavelength is unreasonable: at a wavelength of 282nm, some impurities are not easy to detect

Method used

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  • Method for detecting related substances in Tolterodine tartrate raw material or preparation
  • Method for detecting related substances in Tolterodine tartrate raw material or preparation
  • Method for detecting related substances in Tolterodine tartrate raw material or preparation

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Effect test

Embodiment 1

[0027] Embodiment 1 System suitability, sample determination and forced degradation test thereof

[0028] Instruments and conditions: Waters liquid chromatography system, DAD detector, chromatographic column: Agilent CN (250 × 4.6mm, 5μm); detection wavelength: 215nm; dissolve with phosphate buffer (sodium dihydrogen phosphate 7.8g, add water 1000ml) , add 5ml of triethylamine, adjust the pH to 2.5 with phosphoric acid)-acetonitrile (70:30) as the mobile phase, the detection wavelength is 215nm.

[0029] experiment procedure:

[0030] 1. System suitability test: take tolterodine tartrate and impurity A (N, N diisopropyl-3-(2-methoxy-5 methylphenyl)-3-amphetamine fumarate) Appropriate amount, accurately weighed, add acetonitrile-water (3:7) to dissolve and dilute to make a mixed solution containing 0.25mg per 1ml, accurately measure 10μl and inject it into the liquid chromatograph, record the chromatogram, see the attached figure 1 .

[0031] Depend on figure 1 It can be se...

Embodiment 2

[0043] Embodiment 2 Sensitivity, formulation specificity and sample determination experiment

[0044] Instruments and conditions: Agilent 1200 liquid chromatography system, DAD detector, chromatographic column: Agilent CN (250×4.6mm, 5μm); detection wavelength: 215nm; use phosphate buffer (7.8g sodium dihydrogen phosphate, add water 1000ml to make Dissolve, add 5ml of triethylamine, adjust the pH to 2.5 with phosphoric acid)-acetonitrile (70:30) as the mobile phase, and the detection wavelength is 215nm.

[0045] 1. Sensitivity test: Take an appropriate amount of tolterodine tartrate reference substance, add acetonitrile-water (3:7) to gradually dilute to make a solution containing 0.25 μg (0.05%) and 0.05 μg (0.01%) in every 1 ml, and accurately measure Take 10 μl and check according to the law, the results are shown in the attached Figure 6 , 7 .

[0046] Depend on Figure 6 , Figure 7It can be seen that when the concentration is 0.25 μg / ml, the signal-to-noise ratio ...

Embodiment 3

[0051] Embodiment 3 method durability test

[0052] Agilent 1200 liquid chromatography system, VWD detector, chromatographic column: Agilent CN (250×4.6mm, 5μm); detection wavelength: 215nm; dissolve with phosphate buffer (6.8g potassium dihydrogen phosphate, add water 1000ml, add three Ethylamine 5ml, adjust pH to 3.0 with phosphoric acid)-acetonitrile (80:20) as mobile phase, detection wavelength is 215nm. Take tolterodine tartrate and impurity A (N, N diisopropyl-3-(2-methoxyl-5 methylphenyl)-3-amphetamine fumarate) each appropriate amount, accurately weighed, add Dissolve and dilute acetonitrile-water (2:8) to make a mixed solution containing 0.25 mg per 1 ml, accurately measure 10 μl of the solution and inject it into a liquid chromatograph, record the chromatogram, and separate tolterodine tartrate from impurity A Degree should be greater than 10, and the tailing factor of tolterodine tartrate peak should be less than 2.0.

[0053] System suitability test: take toltero...

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Abstract

The invention relates to a method for detecting related substances in a Tolterodine tartrate raw material or preparation. The method employs high performance liquid chromatography (HPLC) for diction, adopts chromatographic column filled with cyano bonds and silica gel as an immobile phase, and takes a mixed solution of a phosphate buffer and acetonitrile. And the detection wavelength is 215nm. The method of the invention can effectively separate Tolterodine tartrate and other impurities well, detects impurities comprehensively within 215nm, and accurately determines the content of other impurities. Also, the method provided in the invention has the characteristics of simple operation, high sensitivity, accurate and reliable result as well as strong specificity.

Description

technical field [0001] The invention relates to a method for detecting related substances of tolterodine tartrate raw materials or preparations. Background technique [0002] Tolterodine is a competitive M receptor antagonist, and its selectivity to the bladder is significantly stronger than that to the salivary glands, and its inhibition of bladder contraction is about 20 times that of the salivary glands. For the treatment of urinary incontinence, urinary frequency and urgency caused by bladder irritation. [0003] At present, the determination methods for related substances of tolterodine tartrate raw materials and preparations have been recorded in the national standard, and the quality standard numbers are WS1-(X-181)-2003Z and WS1-(X-182)-2003Z respectively. The determination method uses methanol-phosphate buffered saline (take 500ml of water, add 3ml of phosphoric acid, adjust the pH value to 7.2 with diethylamine) (80:20) as the mobile phase, and the detection wavel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/60
Inventor 赵志全刘阿利崔祥祯
Owner LUNAN PHARMA GROUP CORPORATION
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