Method for detecting Tadalafei and derivative thereof

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

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

CN101021482AActive Publication Date: 2007-08-22BEIJING INST FOR DRUG CONTROL
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  • Method for detecting Tadalafei and derivative thereof
  • 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 sulfuric acid (obtained by the reaction of sodium molybdate and sulfuric acid) to produce a blue-purple solution. Although there are some other specific alkaloids that can undergo Frhde reaction, the color of the resulting solution is different due to the difference in structure. The reaction colors of other specific alkaloids Frhde are shown in Table 1:

[0025] Table 1: Reaction colors of other specific alkaloids Frhde

[0026] Alkaloids

Color rendering

Alkaloids

Color rendering

morphine

Purple→brown green

Emetine

dark green

codeine

green → blue

strychnine

red purple

Ethylmorphine

green → blue

Colchicine

yellow green

Apomorphine

purple → green

Aconitine

yellow

Narcotine

green → red yellow

Toxicine

colorless → yellow

...

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 finel...

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, and its derivatives mainly contain methyl groups on N-heterocycles surrounded by amino groups (-NH 2 ) is substituted, see formula II; and the methyl group on the N-containing heterocycle is ethyl (-CH 2 CH 3 ), hydroxymethyl (-CH 2OH) 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]

[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] [0004] At present, there is no rapid test method for tadala...

Claims

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Application Information

Patent Timeline
22 Aug 2007
Publication
CN101021482A
IPC
G01N21/78; G01N33/15; G01N1/28
Inventors
高青; 张喆