Method for detecting Tadalafei and derivative thereof

A technology for tadalafil and its derivatives, which is applied in the field of detection of tadalafil and its derivatives, can solve the problems of lack of inspection equipment, difficulty in screening, and inability to identify new derivatives, and achieve strong specificity, sensitive response, The effect of high accuracy

Active Publication Date: 2007-08-22
BEIJING INST FOR DRUG CONTROL
View PDF0 Cites 15 Cited by
  • 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

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1, the method for detecting tadalafil and its derivatives

[0022] The specific operations of the method for detecting tadalafil and derivatives thereof of the present invention are as follows:

[0023] 1. Sampling volume

[0024] For different types of samples to be tested, the recommended sampling volume is shown in Table 1 below.

[0025] Table 1 Recommended sampling table

[0026] dosage form

Sampling volume

tablet

1

capsule

Contents of 1 capsule

honey pill

1 / 4 pill

single dose oral solution

1 / 2 stick

other solid

0.1-0.2g

[0027] 2. Preparation of the test article

[0028] Preparation of solid test sample Add 5-10ml chloroform to the finely ground or chopped sample, grind to dissolve, filter with filter paper moistened with chloroform in advance, put the filtrate in a white porcelain evaporating dish, evaporate to dryness in a water bath at 80°C or use a hair dryer Blow d...

Embodiment 2

[0038] Embodiment 2, the accuracy test that the inventive method detects tadalafil

[0039] 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, announced on March 14, 2006), HPLC-MS-MS Methods Check tadalafil, sildenafil citrate, vardenafil hydrochloride, the results are shown in Table 3.

[0040] Table 3: Test results of multiple batches of samples

[0041] 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 *

sample 3

pill

1 pill

yellowish brown

Does not contain *

Sample 4

piece

1 piece finely powdered

yello...

Embodiment 3

[0046] Embodiment 3, the method of the present invention detects tadalafil derivatives

[0047] The method of the present invention can not only detect tadalafil, but also detect tadalafil derivatives, and its derivatives mainly contain methyl groups on N-heterocycles surrounded by amino groups (-NH 2 ) is substituted, see formula II (aminotadalafil); and the methyl group on the N-containing heterocycle is replaced by ethyl (-CH 2 CH 3 ), 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.

[0048] (Formula II)

[0049] For the detection of capsule samples containing tadalafil derivatives with the structure of formula II by HPLC-MS-MS method, the content of 1 capsule was taken for detection, and the color development result was blue-purple, which was a positive result.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a method to detect Tadalafil and its derivative. It contains steps: (1) Color reaction. Make color reaction by adding concentrated sulfuric acid. (2) Result estimation. If color reaction presents blue violet, there are Tadalafil and its derivative in test samples. The method 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): G01N21/78G01N33/15G01N1/28
Inventor 高青张喆周立春代红车宝泉王志斌赵明方颍郭洪祝
Owner BEIJING INST FOR DRUG CONTROL
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap