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Method for detecting Tadalafei and derivative thereof

A technology for tadalafil and its derivatives, applied in the field of detection of tadalafil and its derivatives, can solve the problems of difficult identification, failure to identify new derivatives, lack of testing equipment, etc., and achieve strong specificity, sensitive response, The effect of high accuracy

Active Publication Date: 2010-02-10
BEIJING INST FOR DRUG CONTROL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there is no rapid test method for tadalafil released in the food and drug testing industry. For pharmacies and grassroots drug control institutes, due to the lack of advanced testing equipment, it is difficult to identify whether food, traditional Chinese medicine preparations and health foods contain prohibited drugs. Therefore, the establishment Simple, accurate and fast identification method has special significance
In addition, some manufacturers continue to manufacture derivatives of the above-mentioned compounds in order to evade the inspection of law enforcement agencies, and new derivatives cannot be identified even by relying on HPLC methods

Method used

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  • Method for detecting Tadalafei and derivative thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1, the method for detecting tadalafil

[0023] Principle of the method:

[0024] Tadalafil can react with molybdenum sulfate (obtained from the reaction of sodium molybdate and sulfuric acid) (Fellerd) reaction to produce a blue-violet solution. Although some other specific alkaloids can also occur reaction, but the color of the resulting solution is different due to the difference in structure. other specific alkaloids The reaction color is shown in Table 1:

[0025] Table 1: Other specific alkaloids Reactive color

[0026]

[0027] The reaction is specific for morphine alkaloids, The color formed by the reaction is obviously different depending on the structural difference of such alkaloids (see Table 1); and most alkaloids The reaction color is a gradual process, such as reserpine, which quickly changes from yellow to blue after adding 0.1% sodium molybdate sulfuric acid solution, and tadalafil, blue-purple can be stable for a long time;...

Embodiment 2

[0045] Embodiment 2, the accuracy test that the inventive method detects tadalafil

[0046] Commercially available 39 batches of samples are detected by the method of the present invention, meanwhile, according to the State Drug and Food Administration drug inspection supplementary inspection method and inspection item approval document (2006009, released on March 14th, 2006), HPLC-MS-MS Methods Check tadalafil, sildenafil citrate, vardenafil hydrochloride, the results are shown in Table 3.

[0047] Table 3: Test results of multiple batches of samples

[0048] product name

dosage form

Sampling volume

Color rendering result

mass spectrometry results

sample 1

capsule

Contents of 1 capsule

blue-purple

tadalafil

sample 2

pill

1 pill

yellowish brown

Does not contain*

[0049] sample 3

pill

1 pill

yellowish brown

Does not contain*

Sample 4

piece

1 piece finely powd...

Embodiment 3

[0054] Embodiment 3, the method of the present invention detects tadalafil derivatives

[0055] The method of the present invention can not only detect tadalafil, but also detect tadalafil derivatives. 2 ) is substituted, see formula II; and the methyl group on the N-containing heterocycle is ethyl (-CH 2 CH3 ), hydroxymethyl (-CH 2 OH) substituted derivatives. The process of detecting tadalafil derivatives is the same as that of tadalafil, and the judgment of positive results is also the same.

[0056] (Formula II)

[0057] For the HPLC-MS-MS method to detect the capsule sample containing the tadalafil derivative (aminotadalafil) with the structure of formula II, take the contents of 1 capsule for detection, and the color development result is blue-purple, which is a positive result.

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Abstract

The invention discloses a method to detect Tadalafil and its derivative: (1) Color reaction. Make color reaction by adding vitriol solution of sodium molybdate. (2) Result estimation. If color reaction presents blue violet, there are Tadalafil and its derivative in test samples. The method adopts special Flood reaction of Tadalafil is for testing, which has merits of quick, simple, high sensitivity and strong property etc.

Description

technical field [0001] The invention relates to a method for detecting tadalafil and its derivatives. Background technique [0002] Tadalafil is a second-generation phosphodiesterase inhibitor developed by Eli Lilly and Company of the United States. It is clinically used to treat male erectile dysfunction (ED). Its structural formula is shown in formula I, and its molecular formula is C 22 h 19 N 3 o 4 , the trade name is Cialis, which is a prescription drug. Compared with the other two drugs for treating ED, sildenafil and vardenafil, tadalafil has a rapid onset of action and a long duration of action. It has been detected in food, aphrodisiac Chinese medicine preparations or health food for many times, and even The detection of its derivatives is self-evident to the harm of uninformed consumers, and also caused confusion in the market of traditional Chinese medicine preparations and health food. [0003] (Formula I) [0004] At present, there is no rapid test metho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/78G01N33/15G01N1/28
Inventor 高青张喆车宝泉周立春代红王志斌赵明方颍郭洪祝
Owner BEIJING INST FOR DRUG CONTROL