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
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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 Frhde reaction, the color of the resulting solution is different due to the difference in structure. The reaction colors of other specific alkaloids Frhde are shown in Table 1:
[0025] Table 1: Reaction colors of other specific alkaloids Frhde
[0026] Alkaloids
Color rendering
Alkaloids
Color rendering
Purple→brown green
Emetine
dark green
green → blue
red purple
Ethylmorphine
green → blue
yellow green
purple → green
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
Sampling volume
Color rendering result
mass spectrometry results
sample 1
Contents of 1 capsule
blue-purple
tadalafil
sample 2
1 pill
yellowish brown
Does not contain *
[0049] sample 3
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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