CN102735709A - Method for rapidly detecting sildenafil citrate illegally added in health food products and traditional Chinese medicine preparations - Google Patents
Method for rapidly detecting sildenafil citrate illegally added in health food products and traditional Chinese medicine preparations Download PDFInfo
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- CN102735709A CN102735709A CN2012102235089A CN201210223508A CN102735709A CN 102735709 A CN102735709 A CN 102735709A CN 2012102235089 A CN2012102235089 A CN 2012102235089A CN 201210223508 A CN201210223508 A CN 201210223508A CN 102735709 A CN102735709 A CN 102735709A
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Abstract
The invention discloses a method for rapidly detecting sildenafil citrate illegally added in health food products and traditional Chinese medicine preparations. The technical scheme adopted by the invention is that: differential scanning calorimetric analysis technology is utilized, and sildenafil citrate added in a sample is detected. Compared with prior arts, the method provided by the invention is advantaged in short analysis time, good repeatability, low cost, high specificity, and high accuracy. With the method, the sample can be detected rapidly and accurately. Therefore, daily supervision can be conveniently carried out, and public drug-use safety and physical health can be ensured.
Description
Technical field
The present invention relates to a kind of detection method, relate in particular to a kind of illegal method for quick that adds sildenafil citrate in health food and the Chinese medicine preparation that detects.
Background technology
Rising in recent years Chinese medicine heat, it is conventionally believed that Chinese medicine can effect a permanent cure, and toxic and side effect is little.Some illegal enterprises are through the illegal Western medicine that adds in tonifying kidney and strengthening yang class Chinese medicine preparation, thus the increase curative effect, the deception consumer.There is randomness in illegal the interpolation, and dosage is the amount doesn't matter, even is that simple emphasical curative effect severe overweight, this type of medicine do not pass through the strict clinical trial and the detection of bad reaction, and potential is very harmful, seriously can cause death; The illegal in addition material that adds influences each other with the traditional Chinese medicine ingredients of complicacy probably and acts on, and increases the probability of bad reaction greatly.
Sildenafil citrate also is " viagra "; Principal ingredient and chemical name are: [[5-(6 for 4-ethoxy-3-for 1-; 7-dihydro-1-methyl-7-oxo-3-propyl group-1H-pyrazolo [4; 3d] pyrimidine)] benzene sulfonyl]-4-methyl piperazine citrate, its structural formula is like (I), and U.S. food and drug administration (FDA) are in the special-purpose medicaments of this medicine of official approval on March 27 in 1997 as the treatment impotence.
Pharmacodynamics shows, behind oral this medicine of healthy male patient, causes the clinostatism blood pressure drops, and 1～2 hour blood pressure drops in back is the most obvious taking medicine.American heart institute and american heart association have spelt out and have used pernitric acid esters medicine person to forbid silaenafil in 24 hours.But because the specific use and the added value of this product are higher; And silaenafil is cheap now, so illegally in tonifying kidney and strengthening yang class Chinese patent drug, health food add sildenafil citrate to produce the phenomenon of the Medicines and Health Product of quick-acting tonifying kidney and strengthening yangs at a low price startling.
In the prior art; Illegal detection method of adding sildenafil citrate in health food, the Chinese medicine preparation is mainly high performance liquid chromatography and LC-MS method; All need sample is carried out pre-treatment; Detection time is longer relatively, and detection need be done the contrast of standard items simultaneously at every turn, so has increased the detection cost.During 12; Guarantee that people's diet drug safety has become the major tasks of government and all departments of medicine inspection system; In the face of the market environment that becomes increasingly complex, the raising of fraud means needs to set up the method that fast and accurately a large amount of samples is detected and judge.
Summary of the invention
Illegal method of adding sildenafil citrate in the fast detecting health food that the purpose of this invention is to provide that a kind of specificity is strong, analysis time is short, accuracy is high, good reproducibility and cost is low, the Chinese medicine preparation.
For realizing that the technical scheme that above-mentioned purpose the present invention adopts is: illegal method of adding sildenafil citrate in a kind of fast detecting health food, the Chinese medicine preparation; Adopt the differential scanning calorimetric analysis method; Sample is measured; Step is following: sample is placed differential scanning calorimetric analysis, is 10 ℃ of min with heating rate
-1, 150 ℃～250 ℃ scopes, carrying out differential scanning calorimetric analysis, the record collection of illustrative plates calculates the onset value.
Criterion is: getting the sildenafil citrate reference substance, is 10 ℃ of min with heating rate
-1, 150 ℃～250 ℃ scopes, it being carried out differential scanning calorimetric analysis, the record collection of illustrative plates calculates the onset value.The onset value of testing sample and the onset value of reference substance are compared, the onset value of sample reference substance ± 5 ℃ of scopes in, then judge and contain sildenafil citrate in the sample.
Method of the present invention is applicable to tonifying kidney and strengthening yang class health food, or tablet, hard capsule and pill etc. in the Chinese medicine preparation.
The present invention compared with prior art has following advantage:
(1) specificity is strong: fusing point is the physics and chemistry attribute of material, has very strong specificity.
(2) do not need pre-treatment: technology such as no matter chemical discriminating, thin layer, high performance liquid chromatography, LC-MS; All need sample is carried out pre-treatment in various degree; And adopt method of the present invention, testing sample not to need any pre-treatment, significantly reduced analytical procedure, time and human resources.
(3) analysis time is short: existing method all needs the suitable time to be used for the preparation of instrument and the analysis of sample, adopts method of the present invention, only needs 10 minutes can obtain the result.
(4) good reproducibility: existing chromatography is because condition effect such as developping agent, moving phase, chromatographic columns; The Rf value or the appearance time of testing sample all are not quite similar at every turn; And the result of the inventive method only depends on the physical characteristics of sildenafil citrate self; After heating rate is confirmed, there is not influence to measuring the result between different experiments personnel, different experiments chamber.
(5) cost is low: the present invention does not need any reagent and accessory; And because its specificity is strong, good reproducibility, so after only need setting up the contrast collection of illustrative plates of a sildenafil citrate, other checks need not used reference substance; Save the use of reference substance, reduced the detection cost.
(6) accuracy good: adopt method of the present invention, confirm that through 76 routine experimental results further being carried out the LC-MS method accuracy rate is 100%, the non-false positive phenomenon.
(7) social benefit is good: from the food and drug safety angle; Can exercise supervision, check and investigate and prosecute the illegal interpolation in establishing-Yang class health food and the Chinese medicine preparation fast and accurately, guarantee broad masses of the people's diet drug safety and healthy.
Description of drawings
Fig. 1 is a sildenafil citrate reference substance differential scanning calorimetric thermogram.
Fig. 2 is in the testing sample, the positive differential scanning calorimetric thermogram.
Fig. 3 is in the testing sample, the negative sample differential scanning calorimetric thermogram.
Fig. 4 is the differential scanning calorimetric thermogram of self-control positive.
Embodiment
Illegal method of adding sildenafil citrate in 1 one kinds of fast detecting health foods of embodiment, the Chinese medicine preparation
Step is following:
1. getting the about 15mg of sildenafil citrate reference substance, is 10 ℃ of min with heating rate
-1, 150 ℃～250 ℃ scopes, it is carried out differential scanning calorimetric analysis, the record collection of illustrative plates, as shown in Figure 1, calculating its onset value is 195.383 ℃.
2. tonifying kidney and strengthening yang class health food and the Chinese medicine preparation (tablet and capsule and pill) of collecting 76 different manufacturers from market are as testing sample.Getting the about 15mg of fine powder of testing sample, is 10 ℃ of min with heating rate
-1, 150 ℃～250 ℃ scopes, it being carried out differential scanning calorimetric analysis, the record collection of illustrative plates calculates the onset value.Fig. 2 is the differential scanning calorimetric thermogram of the 1st routine sample, and its onset value is 193.947 ℃; Fig. 3 is the differential scanning calorimetric thermogram of the 5th routine sample, no endothermic peak.The collection of illustrative plates of all the other samples omits.
3. criterion: the onset value of testing sample and the onset value of reference substance are compared, the onset value of sample reference substance ± 5 ℃ of scopes in, then judge and contain sildenafil citrate in the sample.
4. testing result: the positive sample of the 1st routine sample, the negative sample of the 5th routine sample.Through detecting, positive is 31 in the 76 routine samples, and negative sample is 45.
5. demonstration test:
1. get the 5th routine negative sample, add the sildenafil citrate reference substance, as the self-control positive.With heating rate is 10 ℃ of min
-1, 150 ℃～250 ℃ scopes, it is carried out differential scanning calorimetric analysis, the record collection of illustrative plates, as shown in Figure 4, calculating its onset value is 193.018 ℃.
2. simultaneously above-mentioned 76 samples are carried out the LC-MS analytical technology and testing result of the present invention compares, as a result rate of accuracy reached to 100%.
It is thus clear that, of the present invention based on the differential scanning calorimetric analysis technology can rapid screening tonifying kidney and strengthening yang class health food and Chinese medicine preparation in the illegal sildenafil citrate that adds.Method of the present invention can satisfy technical requirement fast and accurately.
Claims (2)
1. illegal method of adding sildenafil citrate in a fast detecting health food, the Chinese medicine preparation; It is characterized in that: adopt the differential scanning calorimetric analysis method; Sample is measured, and step is following: sample is placed the differential scanning calorimetric analysis appearance, is 10 ℃ of min with heating rate
-1, 150 ℃～250 ℃ scopes, carrying out differential scanning calorimetric analysis, the record collection of illustrative plates calculates the onset value.
2. according to the described method of claim 1, it is characterized in that: described sample is a tonifying kidney and strengthening yang class health food, or tablet, hard capsule and pill in the Chinese medicine preparation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210223508.9A CN102735709B (en) | 2012-07-02 | 2012-07-02 | Method for rapidly detecting sildenafil citrate illegally added in health food products and traditional Chinese medicine preparations |
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| CN201210223508.9A CN102735709B (en) | 2012-07-02 | 2012-07-02 | Method for rapidly detecting sildenafil citrate illegally added in health food products and traditional Chinese medicine preparations |
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| CN102735709A true CN102735709A (en) | 2012-10-17 |
| CN102735709B CN102735709B (en) | 2015-01-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110174438A (en) * | 2019-07-04 | 2019-08-27 | 云南中烟工业有限责任公司 | A kind of method of nicotine in quick identification tobacco juice for electronic smoke |
Citations (4)
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| US6406918B1 (en) * | 1999-01-25 | 2002-06-18 | University Of Massachusetts | Thermal analysis for detection and identification of explosives and other controlled substances |
| CN1563953A (en) * | 2004-03-24 | 2005-01-12 | 广东省药品检验所 | Fast analyzing method for sildenafil citrate doped medicine, health products and foods |
| CN101021479A (en) * | 2007-03-20 | 2007-08-22 | 北京市药品检验所 | Method for assaying cedinafei and derivative thereof |
| CN101078697A (en) * | 2007-06-29 | 2007-11-28 | 南京师范大学 | Method for determining phase change temperature of liposome |
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2012
- 2012-07-02 CN CN201210223508.9A patent/CN102735709B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6406918B1 (en) * | 1999-01-25 | 2002-06-18 | University Of Massachusetts | Thermal analysis for detection and identification of explosives and other controlled substances |
| CN1563953A (en) * | 2004-03-24 | 2005-01-12 | 广东省药品检验所 | Fast analyzing method for sildenafil citrate doped medicine, health products and foods |
| CN101021479A (en) * | 2007-03-20 | 2007-08-22 | 北京市药品检验所 | Method for assaying cedinafei and derivative thereof |
| CN101078697A (en) * | 2007-06-29 | 2007-11-28 | 南京师范大学 | Method for determining phase change temperature of liposome |
Non-Patent Citations (2)
| Title |
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| 林锦明 等: "热分析技术在药学领域中的应用", 《第二军医大学学报》 * |
| 金宏 等: "差示扫描量热法鉴别药用高密度聚乙烯瓶中掺杂聚丙烯", 《药物分析杂志》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110174438A (en) * | 2019-07-04 | 2019-08-27 | 云南中烟工业有限责任公司 | A kind of method of nicotine in quick identification tobacco juice for electronic smoke |
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| CN102735709B (en) | 2015-01-07 |
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