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UV spectrophotometry and HPLC combined method for determining content of phenylpropanol

A technology of high performance liquid chromatography and determination method, which is applied in the field of combined determination of phenylpropanol content by ultraviolet spectrophotometry and high performance liquid chromatography, and can solve the problem of inappropriate selection of buffer solution to stabilize the acidity of medium and detection wavelength and ineffective application. Measurement, not considering, etc.

Inactive Publication Date: 2007-05-23
NANJING NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN1588043A (application number 200410050273.3) and Journal of China Three Gorges University (Natural Science Edition) 2005,27 (3): 274-282 adopt strong selectivity, good high performance liquid chromatography of separation degree to measure phenylpropanol, and this method is applied to The determination of the content of preparations prepared from phenylpropanol raw materials or a single batch of excipients has a good effect, but the main problems of this method are that the buffer solution is not used to stabilize the acidity of the medium and the detection wavelength is not properly selected.
What is more important in addition is that this method determines that the maximum absorption of the main impurity propiophenone that needs to be detected is not considered to be 208nm, 242nm and the feature of 244nm, so that the preferred 215 ± 1nm or 257 ± 1nm of this method is in the slope of the propiophenone absorption curve. At the large peak shoulder, the result further increases the inaccuracy of the detection results of propiophenone in the purity determination, and the detection results with large fluctuations cannot be used normally
Jiangsu Pharmacy and Clinical Research, 2004, 12 (4): 25 has reported the method that ultraviolet spectrophotometry measures phenylpropanol capsule content, and this method is that medium measures phenylpropanol with ethanol, because cyclodextrin and various solid excipients Insoluble, this method cannot be effectively applied to the determination of phenylpropanol solid preparations

Method used

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  • UV spectrophotometry and HPLC combined method for determining content of phenylpropanol
  • UV spectrophotometry and HPLC combined method for determining content of phenylpropanol
  • UV spectrophotometry and HPLC combined method for determining content of phenylpropanol

Examples

Experimental program
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Effect test

Embodiment 1

[0102] Example 1: Accurately weigh 110 mg of phenylpropanol and 935 mg of β-CD (1:1 mol) into a 100 ml volumetric flask, add 0.1% phosphate buffer with pH=6.86 to constant volume, and ultrasonic treatment for 30 minutes, which is 1.10 mg / ml Standard solution of phenylpropanol solution. Dilute by 20, 10, 5, 2.5, and 2 times, and take the average of three measurements at each point to obtain the standard curve of phenylpropanol under the condition of β-CD containing the prescribed dose: A = 1.5256C + 0.0656, r = 0.9999.

[0103] Take phenylpropanol tablets (batch number 050516), crush into fine powder, accurately weigh 65mg, sonicate with 20ml of phosphate buffer solution for 30min, dilute to 25ml, and prepare a solution containing about 0.26mg / ml of phenylpropanol at 257nm The absorbance was measured, A = 0.4620, and the calculated content of phenylpropanol was 99.55% (labeled amount in phenylpropanol tablets).

Embodiment 2

[0104] Example 2: Basically the same as Example 1, but adding 0.5% acetic acid-sodium acetate buffer with pH=4.02 to make the volume constant to obtain a standard curve of phenylpropanol under the condition of β-CD containing the prescribed dose: A=1.4996C+0.1733, r = 0.9987. The absorbance was measured at 257nm, A=0.5632, and the calculated content of phenylpropanol was 99.61%.

[0105] Determination

[0106] The peak area ratio of phenylacetone to phenylpropanol=0.28, which is less than 1.98 (the content of phenylacetone is 0.99%). The content of phenylacetone in batch number 050516 phenylpropanol tablets is less than 1%, and the sample is qualified.

[0107] Determination

[0108] The peak area ratio of phenylacetone to phenylpropanol=0.30, which is less than 2.33 (the content of phenylacetone is 0.99%). The content of phenylacetone in batch number 050516 phenylpropanol tablets is less than 1%, and the sample is qualified.

Embodiment 5

[0109] Example 5: Basically the same as Example 2, but adding 0.5% phosphate buffer solution with pH=5.00 to make the volume constant.

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Abstract

The invention relates to detecting the alcohol-within-benzene content jointly using UV spectrophotometry method and HPLC method, and the method is aimed at the quality control to the phenylpropanol content and impurities of the drug; the quality control method of the phenylpropanol and its preparation in the invention includes the content detection method of phenylpropanol and effective phenylpropanol component of preparation, and the impurities content detection method of phenylpropanol and its preparation; among them, the content detection method of phenylpropanol and effective phenylpropanol component of preparation in the invention has the following steps: a. the preparation of standard solution, b. the preparation of the testing solution, c. standard curve mapping, d. sample content detection using UV spectrophotometry, with 60:40 phosphate water buffer solution as the solvent, at 257nm wavelength to measure absorbance, and according to the absorbance calculating the sample content.

Description

Technical field: [0001] The invention relates to a method for determining the content and impurities of phenylpropanol by combining ultraviolet spectrophotometry and high performance liquid chromatography. The method aims at quality control of the content of phenylpropanol and impurities in medicines. Background technique: [0002] Phenylpropanol, commonly known as cholestrol, is a clinically used bile secretion enhancer. It was first synthesized by Warrb and Cortese in 1927 and was first marketed in Germany. my country started production in 1977. The product is included in all editions of the National Pharmacopoeia. Phenylpropanol is a white or slightly yellow oily liquid; it has a slight ester odor and a pungent taste. It is easily soluble in methanol, ethanol and chloroform, and slightly soluble in water. Phenylpropanol has definite curative effect and stable market. The clinical dosage form is a capsule, and its solid preparation using cyclodextrin inclusion technology is und...

Claims

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Application Information

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IPC IPC(8): G01N35/00G01N21/33G01N30/74G01N30/02G01N30/26
Inventor 任勇李莉娥符义刚高剑锋刘子列周灿
Owner NANJING NORMAL UNIVERSITY
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