CN110068630A - The detection method of silaenafil impurity 12 in a kind of antifatigue class Chinese patent drug and health food - Google Patents
The detection method of silaenafil impurity 12 in a kind of antifatigue class Chinese patent drug and health food Download PDFInfo
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- CN110068630A CN110068630A CN201910423308.XA CN201910423308A CN110068630A CN 110068630 A CN110068630 A CN 110068630A CN 201910423308 A CN201910423308 A CN 201910423308A CN 110068630 A CN110068630 A CN 110068630A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
The present invention provides a kind of detection methods of silaenafil impurity 12 in antifatigue class Chinese patent drug and health food, carry out screening, chromatographic condition: chromatographic column: C18 chromatographic column using ultra performance liquid chromatography-ultraviolet spectra-time-of-flight mass spectrometry (TOFMS)；Detector: diode array detector；Detection wavelength: 285nm；Scanning wavelength range: 190-400nm；Mobile phase: A-0.1% formic acid solution, B-0.1% formic acid-acetonitrile；Flow velocity: 0.3-0.4mL/min；Column temperature: 25-40 DEG C；Sample volume: 0.1-2 μ L.The method of the present invention is detected using Ultra Performance Liquid Chromatography instrument-diode array detector-time of-flight mass spectrometer, not only can be suitably used for big flux screening, but also be avoided that false positive results；High sensitivity, selectivity is good, saves the time, can be used for illegally adding qualitatively screening, confirmation and the assay of silaenafil impurity 12.
Description
Technical field
The invention belongs to medical detection fields, are related to the detection method of chemicals, and in particular in a kind of antifatigue class at
The detection method of silaenafil impurity 12 in medicine and health food.
Background technique
Silaenafil impurity 12(molecular formula: C25H34N6OS2, molecular weight: 498.2) being the analogue of silaenafil,
It is PDE-5 inhibitor, there is structure parent nucleus identical with silaenafil (see following structural formula), it may have similar pharmacology is made
With, it may be added to by criminal in antifatigue class health food or Chinese patent drug, due to its structure novel, there is no common name,
It is fresh studies have reported that.
Currently, discovery has this substance of addition in the antifatigue class health food in market and Chinese patent drug supervision and inspection, but without
To the high resolution mass spectrum rapid screening of this substance, quantitative approach, the measurement of that non-substance in national issuing standard food
High resolution mass spectrum qualitative checking method in (BJS 201805) containing this substance, but analysis time reaches 20min, and without purple
External spectrum identifies and quantitative approach.So to establish 12 rapid ultra high effect liquid phase chromatogram of silaenafil impurity-ultraviolet-high by the present invention
The Resolution Mass Spectrometry method of inspection, and methodology validation is carried out, identify (10min) for the fast qualitative to this substance to realize, contains
It is fixed to measure.
Summary of the invention
Technical problems to be solved: the object of the present invention is to provide one kind in antifatigue class Chinese patent drug and health food
Add the method for inspection of silaenafil impurity 12, the principle of this method are as follows: test sample is extracted and diluted, C18 chromatography with acetonitrile
Post separation is confirmed according to chromatographic behavior, ultraviolet feature, mass spectrum rule synthesis, establishes quantitative approach using LC-MS.
Technical solution: the detection method of silaenafil impurity 12 in a kind of antifatigue class Chinese patent drug and health food, including it is following
Step:
(1) chromatographic condition:
Chromatographic column: C18 chromatographic column, 100mm/50mm × 2.1mm, 1.7 μm/1.8 μm；
Detector: diode array detector；
Detection wavelength: 285nm；
Scanning wavelength range: 190-400nm；
Mobile phase: 0.1% formic acid solution of A-, 0.1% formic acid of B--acetonitrile；
Flow velocity: 0.3-0.4mL/min；
Column temperature: 25-40 DEG C；
Sample volume: 0.1-2 μ L；
Gradient program: 0-2min, 10%B；7-9min, 90%B；9.1-10min, 10%B；
Mass Spectrometry Conditions:
Electron spray positive ion mode；
Capillary voltage: 3500V；
Dry gas stream amount: 10.0L/min；
Atomization gas pressure: 40psig；
Dry temperature degree: 350 DEG C；
Fragmentation voltage: 100-150 V；
Scanning mode: full scan level-one, second order ms；
Acquisition mode: target MS；
Parent ion: 499.2320；
Collision energy: 20V, 30V；
Scanning of the mass spectrum range: 50-1700；
(2) precision weighs 12 reference substance 10mg of silaenafil impurity, is placed in 10mL volumetric flask, with acetonitrile dissolved dilution to quarter
Degree, as stock solution, then pipettes 0.5mL solution and is placed in 100mL volumetric flask, with acetonitrile dissolved dilution to scale, be made into containing 5 μ
The reference substance solution of g/mL；
(3) fine powder is made in test sample, be uniformly mixed, precision weighs a dose, is placed in 10mL volumetric flask, adds acetonitrile
6mL, vortex 1min, ultrasonic extraction 15min, standing are let cool, and add acetonitrile to scale, supernatant 1.0mL is taken to be placed in 10mL volumetric flask
In, acetonitrile is added to scale, shakes up, membrane filtration, sample introduction, measures；
(4) qualitatively screening is carried out using ultra performance liquid chromatography-ultraviolet spectra-time-of-flight mass spectrometry (TOFMS), take respectively blank solution,
Test solution and control solution, inject LC-MS instrument, according in step (1) chromatography, Mass Spectrometry Conditions detection west ground that
Non- impurity 12.
As a result judge:
In sample chromatogram figure, if there is consistent with 12 retention time of reference substance of silaenafil impurity, ultra-violet absorption spectrum
Peak, then carry out mass spectrum confirmation (extract ion stream chromatogram, level-one parent ion: 499.2320, the main fragment of second order ms:
468.1885,428.1573,371.0994,343.0686,72.0808).If Information in Mass Spectra is all consistent, it is determined that be added to
Silaenafil impurity 12, continues assay.
If do not occur with the consistent chromatographic peak of 12 retention time of reference substance of silaenafil impurity, carry out mass spectrum screening (extract from
Subflow chromatogram, level-one parent ion: 499.2320, the main fragment of second order ms: 468.1885,428.1573,371.0994,
343.0686,72.0808), if result is feminine gender, it is dense to calculate detection for no addition silaenafil impurity 12 in judgement sample
Degree；If result is the positive, the extension rate of sample in the preparation of upper (3) test sample is adjusted to 10 times, again sample introduction, point
Analysis compares chromatographic retention with 12 reference substance of silaenafil impurity, ultra-violet absorption spectrum, extracts ion stream chromatogram, mass spectrum
I and II ion characteristic, if information is all consistent, it is determined that be added to silaenafil impurity 12, continue assay；Such as
Fruit information is inconsistent, then judgement sample is not detected.
Concentrations:
Detection limit according to the form below 1 calculates concentrations are as follows: sample weighting amount 1g, when extension rate is 100, and concentrations are as follows:
12mg/kg。
Assay:
The range of linearity:
Above-mentioned reference substance solution is pipetted, adding dilution in acetonitrile to be configured to ultimate density is respectively 1.0,2.0,5.0,10,20 μ g/mL
Series standard solution carries out linear fit to concentration (X) with peak area (Y), calculates linear equation and related coefficient (see Table 1).
As the result is shown within the scope of 1.0-20 μ g/mL, linear relationship is good (r > 0.990).
Detection limit, quantitative limit:
After taking reference substance solution negative sample extracting solution to dilute step by step sample introduction measure, respectively with 3,10 times of signal-to-noise ratio when it is corresponding
Each concentration of standard solution is detection limit and quantitative limit, and calculated result is shown in Table 1.
The range of linearity of 1 silaenafil impurity 12 of table, linear equation, related coefficient, detection limit
| Compound | Range of linearity μ g/mL | Linear equation | Correlation coefficient r | Detection limit ng | Quantitative limit ng |
| Silaenafil impurity 12 | 0.5-10 | Y=186729X-247990 | 0.9984 | 0.12 | 0.39 |
Accuracy and precision:
Using the sample of testing result feminine gender as matrix, recovery of standard addition measurement is carried out.Weigh taking dose of certain negative sample
Be placed in 15mL tool plug centrifuge tube in, be separately added into silaenafil impurity 12 standard solution (0.1mg/mL) 0.1mL, 0.2mL,
0.3mL, each concentration is 6 parts parallel, adds acetonitrile to 10mL, preparation of the remainder by test solution in step (3), sample introduction, measurement.
The analysans mass spectrum response for calculating separately the solution and the reference substance solution ratio with concentration, to evaluate the accurate of this method
Degree.The standard solution that precision measurement is 1 μ g/mL with concentration, continuous sample introduction 6 times, measurement, the mass spectrum for calculating determinand retains
Time and mass spectrum response signal calculate separately its mean value and relative standard deviation (RSD), and as a result visible precision is good.
The rate of recovery (n=6) of 2 silaenafil impurity 12 of table
| Final compound concentration (μ g/mL) | Average residence time (min) | RSD(%) | Average recovery rate (%) | RSD(%) |
| 1 | 5.252 | 0.047 | 92.87 | 1.6 |
| 2 | 5.250 | 0.040 | 85.91 | 1.4 |
| 3 | 5.253 | 0.088 | 90.18 | 1.7 |
The precision (n=6) of 3 silaenafil impurity 12 of table
| Compound | Average residence time (min) | RSD(%) | Average peak area | RSD(%) |
| Silaenafil impurity 12 | 5.250 | 0.041 | 35323 | 3.9 |
Matrix effect:
In order to investigate the influence that sample substrate responds target compound mass spectrum, using the extracting solution of negative sample as bare substrate
Solution, addition reference substance solution is appropriate, is configured to the analog sample solution that concentration is 1 μ g/mL, sample introduction measurement, with respective concentration
The response of standard solution compares, and calculates matrix effect.As a result, it has been found that the response of component mass spectrum does not change substantially, matrix effect is small
In 5%.
Repeatability:
Positive test sample (tablet) 1 batch is taken, prepares 6 parts, 1 μ L of sample introduction in parallel by preparation method of test article, calibration curve method measurement
The content RSD of silaenafil impurity 12 is 0.31% in sample, and repetitive test meets the requirements.
Stability:
Taking concentration is that the reference substance solution of 1 μ g/mL is placed in autosampler, is measured in 0,1,2,4,8,12 hour sample introduction, point
Not Ji Suan component response, have good stability as the result is shown.
Further, chromatographic column is ACQUITY UPLC HSS T3,100mm × 2.1mm, 1.8 μ in the step (1)
m。
Further, test sample is tablet, capsule or liquid preparation in the step (3).
Further, the tablet takes Shi Yaoyan to partial size≤180 μm.
Further, incline when the capsule is taken and take content.
Further, filter membrane is 0.22 μm of filter membrane in the step (3).
The utility model has the advantages that
1. it is qualitative, fixed that the present invention is carried out using Ultra Performance Liquid Chromatography instrument-diode array detector-time of-flight mass spectrometer
Amount detection, not only can be suitably used for big flux screening, but also be avoided that false positive results.
2. the method for the present invention high sensitivity, selectivity is good, saves the time, can be used for illegally adding silaenafil impurity 12
Qualitatively screening, confirmation and assay.
3. the method for the present invention is suitable for the detection of solid pharmaceutical preparation, method described in text is equally applicable to fluid sample.
4. the method for the present invention can effectively monitor silaenafil impurity 12, reliable means are provided for supervision.
Detailed description of the invention:
Fig. 1 is 12 reference substance solution of silaenafil impurity in embodiment 1 in 285nm chromatogram.
Fig. 2 is test solution in embodiment 1 in 285nm chromatogram.
Fig. 3 is the uv absorption spectra of 12 reference substance solution of silaenafil impurity in embodiment 1.
Fig. 4 is the uv absorption spectra of test solution in embodiment 1.
Fig. 5 is the extraction ion stream chromatogram (EIC) of 12 reference substance solution of silaenafil impurity in embodiment 1.
Fig. 6 is that test solution extracts ion stream chromatogram (EIC) in embodiment 1.
Fig. 7 is reference substance solution high-resolution first mass spectrometric figure in embodiment 1.
Fig. 8 is test solution high-resolution first mass spectrometric figure in embodiment 1.
Fig. 9 is reference substance solution high-resolution second order ms figure (CE:20V) in embodiment 1.
Figure 10 is test solution high-resolution second order ms figure (CE:20V) in embodiment 1.
Figure 11 is reference substance solution high-resolution second order ms figure (CE:30V) in embodiment 1.
Figure 12 is test solution high-resolution second order ms figure (CE:30V) in embodiment 1.
Specific embodiment
Instrument:
1290 Ultra Performance Liquid Chromatography instrument of Agilent (matches DAD detector)；6538 ESI-Q-TOF/MS mass spectrograph of Agilent
(Agilent, America)；KQ-300 DA type data ultrasonic cleaner (production of Kunshan ultrasonic instrument company)；Milli-Q
Pure water system (Millipore company)；Metler-Toledo electronic balance.
Reagent:
Ultrapure water；Methanol, acetonitrile and formic acid are chromatographically pure；12 reference substance of silaenafil impurity.
Embodiment 1
The detection method of silaenafil impurity 12 in a kind of antifatigue class Chinese patent drug and health food, comprising the following steps:
(1) chromatographic condition:
Chromatographic column: ACQUITY UPLC HSS T3,100mm × 2.1mm, 1.8 μm；Detector: diode array detector；Inspection
Survey wavelength: 285nm；Scanning wavelength range 190-400nm；Mobile phase: A-0.1% formic acid solution, B-0.1% formic acid-acetonitrile；Stream
Speed: 0.3mL/min；Column temperature: 30 DEG C；Sample volume: 1 μ L；Gradient program: 0-2min, 10%B；7-9min, 90%B；9.1-
10min, 10%B；
Mass Spectrometry Conditions:
Electron spray positive ion mode；Capillary voltage: 3500V；Dry gas stream amount: 10.0L/min；Atomization gas pressure: 40psig；
Dry temperature degree: 350 DEG C；Fragmentation voltage: 135V；Scanning mode: full scan level-one, second order ms；Acquisition mode: target
MS；Parent ion: 499.2320, retention time: 5.14min(chromatogram), 5.25min(mass spectrogram)；Collision energy: 20V, 30V；
Scanning of the mass spectrum range: 50-1700；
(2) precision weighs 12 reference substance 10mg of silaenafil impurity, is placed in 10mL volumetric flask, extremely with acetonitrile dissolved dilution
10mL, then 0.5mL solution is taken to be placed in 100mL volumetric flask, with methanol dissolved dilution to scale, sample introduction is analyzed；
(3) the oyster piece pressed candy 10 for taking certain lot number, grinds to partial size≤180 μm, is uniformly mixed, and weighing weighs 1 sheet weight
Powder, be placed in 10mL volumetric flask, add acetonitrile 6mL, vortex 1min, ultrasonic extraction 15min, standing is let cool, add acetonitrile to carve
Degree.It takes supernatant 1.0mL to be placed in 10mL volumetric flask, acetonitrile is added to scale, shakes up, 0.22 μm of membrane filtration, sample introduction point
Analysis.
Acquire data:
The data of comparison step (2) and (3) find there is a chromatography at 5.14min under sample solution liquid chromatogram 285nm wavelength
Peak, it is consistent (see Fig. 1-2) with 12 retention time of silaenafil impurity in step (2).
It was found that step (3) chromatographic peak located consistent with 12 retention time of reference substance of silaenafil impurity in step (2), purple
Outer absorption spectrum is consistent (see Fig. 3-4).
It was found that step (3) compound located consistent with 12 retention time of reference substance of silaenafil impurity in step (2)
Extraction ion stream chromatogram, level-one parent ion, second level daughter ion it is all consistent (see Fig. 5-12).
Judge to contain silaenafil impurity 12 in the oyster piece pressed candy of certain lot number.
According to 2 parts of solution of preparation are extracted under the preparation of test solution in step (3), suitably diluted according to actual concentrations
To the standard curve range of linearity, sample introduction acquires data, response signal is substituted into standard curve, calculates chemical combination in test sample
The content of object, result are 11.63mg/ piece.
Claims (6)
1. the detection method of silaenafil impurity 12 in a kind of antifatigue class Chinese patent drug and health food, it is characterised in that: including
Following steps:
(1) chromatographic condition:
Chromatographic column: C18 chromatographic column, 100mm/50mm × 2.1mm, 1.7 μm/1.8 μm；
Detector: diode array detector；
Detection wavelength: 285nm；
Scanning wavelength range: 190-400nm；
Mobile phase: 0.1% formic acid solution of A-, 0.1% formic acid of B--acetonitrile；
Flow velocity: 0.3-0.4mL/min；
Column temperature: 25-40 DEG C；
Sample volume: 0.1-2 μ L；
Gradient program: 0-2min, 10%B；7-9min, 90%B；9.1-10min, 10%B；
Mass Spectrometry Conditions:
Electron spray positive ion mode；
Capillary voltage: 3500V；
Dry gas stream amount: 10.0L/min；
Atomization gas pressure: 40psig；
Dry temperature degree: 350 DEG C；
Fragmentation voltage: 100-150 V；
Scanning mode: full scan level-one, second order ms；
Acquisition mode: target MS；
Parent ion: 499.2320；
Collision energy: 20V, 30V；
Scanning of the mass spectrum range: 50-1700；
(2) precision weighs 12 reference substance 10mg of silaenafil impurity, is placed in 10mL volumetric flask, with acetonitrile dissolved dilution to quarter
Degree, as stock solution, then pipettes 0.5mL solution and is placed in 100mL volumetric flask, with acetonitrile dissolved dilution to scale, be made into containing 5 μ
The reference substance solution of g/mL；
(3) fine powder is made in test sample, be uniformly mixed, precision weighs a dose, is placed in 10mL volumetric flask, adds acetonitrile
6mL, vortex 1min, ultrasonic extraction 15min, standing are let cool, and add acetonitrile to scale, supernatant 1.0mL is taken to be placed in 10mL volumetric flask
In, acetonitrile is added to scale, shakes up, membrane filtration, sample introduction, measures；
(4) qualitatively screening is carried out using ultra performance liquid chromatography-ultraviolet spectra-time-of-flight mass spectrometry (TOFMS), take respectively blank solution,
Test solution and control solution, inject LC-MS instrument, according in step (1) chromatography, Mass Spectrometry Conditions detection west ground that
Non- impurity 12.
2. the detection of silaenafil impurity 12 in a kind of antifatigue class Chinese patent drug according to claim 1 and health food
Method, it is characterised in that: chromatographic column is ACQUITY UPLC HSS T3,100mm × 2.1mm, 1.8 μm in the step (1).
3. the detection side of silaenafil impurity 12 in a kind of antifatigue class Chinese patent drug according to claim 1 and health food
Method, it is characterised in that: test sample is tablet, capsule or liquid preparation in the step (3).
4. the detection side of silaenafil impurity 12 in a kind of antifatigue class Chinese patent drug according to claim 3 and health food
Method, it is characterised in that: the tablet takes Shi Yaoyan to partial size≤180 μm.
5. the detection side of silaenafil impurity 12 in a kind of antifatigue class Chinese patent drug according to claim 3 and health food
Method, it is characterised in that: the capsule inclines when taking takes content.
6. the detection side of silaenafil impurity 12 in a kind of antifatigue class Chinese patent drug according to claim 1 and health food
Method, it is characterised in that: filter membrane is 0.22 μm of filter membrane in the step (3).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111289670A (en) * | 2020-01-16 | 2020-06-16 | 苏州市药品检验检测研究中心 | Detection method of N-butyl-3- (trifluoromethyl) - α -methylphenethylamine in weight-reducing traditional Chinese medicine and food |
| CN112198243A (en) * | 2020-09-10 | 2021-01-08 | 广州白云山医药集团股份有限公司白云山制药总厂 | Method for detecting sildenafil citrate impurity |
| CN114942279A (en) * | 2022-04-15 | 2022-08-26 | 上海市食品药品检验研究院 | Screening method for illegally added glucocorticoids and analogues thereof in cosmetics |
-
2019
- 2019-05-21 CN CN201910423308.XA patent/CN110068630A/en not_active Withdrawn
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| PAULA PROENÇA ET AL.: "Validated UPLC-MS/MS assay for the determination of synthetic phosphodiesterase type-5 inhibitors in postmortem blood samples", 《JOURNAL OF FORENSIC AND LEGAL MEDICINE》 * |
| 中国食品药品检定研究院: "《食品中那非类物质的测定 BJS201805》", 31 May 2018 * |
| 金绍明 等: "超高效液相色谱-串联质谱法测定酒、牡蛎粉、咖啡中2种那非类物质的含量", 《食品安全质量检测学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111289670A (en) * | 2020-01-16 | 2020-06-16 | 苏州市药品检验检测研究中心 | Detection method of N-butyl-3- (trifluoromethyl) - α -methylphenethylamine in weight-reducing traditional Chinese medicine and food |
| CN112198243A (en) * | 2020-09-10 | 2021-01-08 | 广州白云山医药集团股份有限公司白云山制药总厂 | Method for detecting sildenafil citrate impurity |
| CN114942279A (en) * | 2022-04-15 | 2022-08-26 | 上海市食品药品检验研究院 | Screening method for illegally added glucocorticoids and analogues thereof in cosmetics |
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