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A rapid detection method for adding diclofenac sodium in anti-rheumatic Chinese patent medicine or health food

A technology of diclofenac sodium and health food, which is applied in the direction of material analysis by observing the influence of chemical indicators, and analysis by making materials undergo chemical reactions, which can solve the problems of unsuitable on-site detection and high environmental requirements, and achieve the correct rate High, high sensitivity, strong specific effect

Inactive Publication Date: 2011-12-28
广东省潮州市药品检验所 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above method requires the use of expensive analytical instruments, has high requirements on the environment, and needs to be placed in a fixed position, so it is not suitable for on-site detection with high mobility.

Method used

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  • A rapid detection method for adding diclofenac sodium in anti-rheumatic Chinese patent medicine or health food
  • A rapid detection method for adding diclofenac sodium in anti-rheumatic Chinese patent medicine or health food
  • A rapid detection method for adding diclofenac sodium in anti-rheumatic Chinese patent medicine or health food

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0031] The detection of example 1 capsule

[0032] Sample to be tested: Jiarong Zhuanggu Tongbi Capsules (marked as produced by Minsheng Pharmaceutical Co., Ltd., Taiqian County, Henan Province, batch number 20091108), high performance liquid chromatography-DAD test results: in the chromatogram of the test product, the same as the diclofenac sodium reference substance The same chromatographic peak was shown at the retention time, which was positive and contained diclofenac sodium.

[0033] Detection steps:

[0034] (1) Take 2 samples, add the contents (about 0.5g) to 5mL ethyl acetate, seal tightly, shake vigorously up and down for about 1 minute, let stand for a while, filter, and take the filtrate as the test solution;

[0035] (2) Take 1mL of the solution to be tested in a 10ml test tube, slowly add 1ml of 65% nitric acid solution along the wall of the test tube, let it stand for stratification, and observe after 20-30 seconds;

[0036] Interpretation of results: The lowe...

example 2

[0037] The detection of example 2 pills

[0038] Sample to be inspected: Sciatica pills (labeled under the supervision and production of Xinglin Pharmaceutical Co., Ltd., batch number 090108)

[0039] High-performance liquid chromatography-DAD test result: in the chromatogram of the test product, there is no chromatographic peak display at the same retention time as the diclofenac sodium reference substance, which is negative and does not contain diclofenac sodium.

[0040] The inventive method detects:

[0041] (1) Take 2 pills (about 0.4 g) of the pills, pulverize them, add 5 mL of ethyl acetate, seal them tightly, shake them vigorously up and down for about 1 minute, let stand for a while, filter, and take the filtrate as the liquid to be tested;

[0042] (2) Take 1mL of the solution to be tested in a 10ml test tube, slowly add 1ml of 65% nitric acid solution along the wall of the test tube, let it stand for stratification, and observe after 20-30 seconds;

[0043] Interp...

example 3

[0044] Examination of Example 3 Tablets

[0045] Sample to be tested: Compound Fengshining Tablets (marked as produced by Guangdong Luofushan Pharmaceutical Co., Ltd., batch number L09D090).

[0046] High-performance liquid chromatography-DAD detection result: in the chromatogram of the test product, there is no chromatographic peak display at the peak with the same retention time as the diclofenac sodium reference substance, which is negative and does not contain diclofenac sodium.

[0047] The inventive method detects:

[0048] (1) Take 1 tablet of the pill, remove the sugar coating (about 0.25 g), crush it, add 5 mL of ethyl acetate, seal it tightly, shake it up and down vigorously for about 1 minute, let it stand for a while, filter it, and take the filtrate as the solution to be tested;

[0049] (2) Take 1mL of the solution to be tested in a 10ml test tube, slowly add 1ml of 65% nitric acid solution along the wall of the test tube, let it stand for stratification, and ob...

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Abstract

The invention discloses a rapid detection method for diclofenac sodium added to anti-rheumatic Chinese patent medicines or health foods. The method consists of the following steps: (1) taking a solid sample and adding ethyl acetate to prepare a mass volume concentration of 0.05-0.10g / mL solution, shake to dissolve, filter, and take the filtrate as the test solution; or take a liquid sample, add 2.5-10 times the volume of ethyl acetate to mix, let stand and take the ethyl acetate extract as the test solution; (2) Take 1mL of the solution to be tested, add 1mL of 65% nitric acid solution, and let it stand for stratification. After 20 to 30 seconds, if the lower layer solution turns reddish brown, it is judged that the sample contains diclofenac sodium. The detection method of the present invention is easy to operate, strong in specificity, and rapid in color reaction, and can be applied to rapid on-site detection of whether diclofenac sodium is doped in anti-rheumatic Chinese patent medicines or health foods.

Description

technical field [0001] The invention relates to the detection of non-biological materials by means of precipitation, in particular to the detection of diclofenac sodium in medicines. Background technique [0002] Diclofenac Sodium (Diclofenac Sodium), the chemical name is 2-[(2,6-dichlorophenyl)amino]phenylacetic acid sodium. The structural formula of sodium dichlorophenate is as shown in formula (1), and molecular formula is C 12 h 10 ClN 2 Cl 2 NNaO 2 , the molecular weight is 318.13, and the Cas number is 15307-79-6. Diclofenac sodium is a colorless crystalline powder with a melting point of 283-285°C; easily soluble in ethanol, slightly soluble in water, and insoluble in chloroform. [0003] [0004] Diclofenac sodium is a non-steroidal anti-inflammatory drug, its main mechanism is to exert its antipyretic, analgesic and anti-inflammatory effects by inhibiting the synthesis of central prostaglandins. It can play an anti-inflammatory role by inhibiting the synth...

Claims

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Application Information

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IPC IPC(8): G01N21/78
Inventor 池浩波张梦虹李国毅黄冬梅陈琏
Owner 广东省潮州市药品检验所
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