CN105572242A - Non-target quick screening and detecting method for PDE-5 inhibitor banned drugs in health foods - Google Patents
Non-target quick screening and detecting method for PDE-5 inhibitor banned drugs in health foods Download PDFInfo
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Abstract
The invention belongs to the technical field of detection of unknown components in foods and particularly discloses a non-target quick screening and detecting method for illegally-added male aphrodisiac PDE-5 inhibitor western drugs in health foods. The combination of QuEChERS (quick, easy, cheap, effective, rugged, and safe) technology with ultrasound-assisted extraction technology is used for the first time in extracting PDE-5 inhibitor western drugs in a sample, IDA-MS high resolution mass spectrum technology is used to quickly screen and analyze the illegally-added male aphrodisiac PDE-5 inhibitor western drugs according to accurate parent ion and fragment molecular weights of primary mass spectrum and secondary mass spectrum as well as isotopic peak data, unknown PDE-5 inhibitor western drug ingredients are quantitatively identified without standards, and the multi-flux detection problem due to the quantity of targets is solved.
Description
Technical field
The present invention relates to the unknown composition detection technical field of food, particularly, relate to the non-targeted thing rapid screening detection method of the violated medicine of PDE-5 inhibitor class in a kind of health food.
Background technology
Health food is that in China's traditional habit, one is commonly called as, and academicly address is functional food.The meals of people solve the new nutrition concept of hungry traditional nutrition concept development of having enough to eat and wear to health good for health from general, facilitate functional food and are born and development.First the concept of functional food put forward by the early stage Japan eighties in 20th century the earliest, the functional food development history of three more than ten years, but different nationalities and countries and regions exist very large difference to the understanding of this concept and definition; The current world is generally with the definition of European Union to health (functional) food; Health food refers to if can confirm a kind of food preferably except providing common nutritive validity, a kind ofly can also promote that the mode of body health reduction disease risks affects a based food of one or more the target function in body valuably.Along with the development of health food industry, documents and materials research display health food, the food-safety problem especially adding violated western medicine composition in health-care tonic wine becomes increasingly conspicuous.
In current health food, PDE-5 inhibitor class forbidden drug detection technique has HPLC, GC-MS, LC-MS, NMR, LC-FI-ICR-MS, UPLC-TOF-MS, IMS and euzymelinked immunosorbent assay (ELISA).But existing literature research finds that adding PDE-5 inhibitor class forbidden drug in health food reaches more than 80 kinds, conventional chromatograph joint used mass spectrometric analysis method can not all effectively detect analyzes these forbidden drug compositions.
Summary of the invention
The object of the invention is the above-mentioned deficiency in order to overcome prior art, not having under standard items condition, the non-targeted thing rapid screening detection method of the violated medicine of PDE-5 inhibitor class in a kind of health food is provided.
To achieve these goals, the present invention is achieved by the following technical programs:
In health food, a non-targeted thing rapid screening detection method for the violated medicine of PDE-5 inhibitor class, comprises the steps:
S1. QuEChERS combine with technique ultrasound on extracting technology is adopted to carry out pre-treatment extraction to health food to be measured, extraction conditions is: the solution (the two volume ratio 6:4) adding 15mL acetonitrile and water in 1mL or 1g health food, 1.2g magnesium sulfate and 0.3g sodium chloride spreading agent, 80mg adsorbent C18, vortex, ultrasonic 10 ~ 15min, gets supernatant after centrifugal layering, supernatant constant volume dilutes, get 1mL again dilute after solution cross after organic system filter membrane as extraction sample liquid;
S2. get extraction sample liquid and carry out IDA-MS data acquisition: the condition of IDA-MS Screening analysis is: liquid phase separation condition is mobile phase A is 0.1% aqueous formic acid, Mobile phase B is acetonitrile, flow velocity 0.5mL/min, gradient elution: B phase increases to 30%, 7min by initial volume than 10%, 1min and increases to 60%, 1min is down to 10%, retain 3min, column temperature 40 DEG C, C18 chromatographic column; Gradient elution mode Mass Spectrometry Conditions: ESI and APCI multiple source; Positive ion scan mode; APCI source connects automatic correction system, and sample is ESI Ionization mode, Curtaingas:40psi, ion gun gas1:50psi, ion gun gas2:50psi, ion source temperature 500 DEG C, ion source voltage 5500V; One-level TOF-MS scans exact mass scope: 100 ~ 1000Da, data acquisition time 100ms, DP:100V, CE:10V; Secondary IDA-MS scans exact mass scope: 50 ~ 1000Da, DP:100V, CE:35 ± 15V; Highly sensitive pattern, data acquisition time 50ms, signal threshold value 100cps, IDA test every circle collection 6 secondary data, and dynamic background subtraction is deducted;
S3. the IDA-MS high resolution mass spectrum data analysis of sample, utilizes the process of PeakView data analysis software to obtain accurate molecular masses, isotopic molecule amount, molecular formula, the chromatographic retention of object, and accurate secondary fragment molecular weight; In conjunction with ChemSpider structural database, Qualitative Identification unknown PDE-5 inhibitor class western medicine composition.
The present invention select Vardenafil, pseudo-Vardenafil, sulfo-Ai Dinafei, hydroxyl Acctildenafil, Genedenafil, sulfo-silaenafil, Acctildenafil, person of outstanding talent not silaenafil, silaenafil, hydroxyl person of outstanding talent not silaenafil, Racxanthoabthrafil, tadalafil, amino tadalafil totally 13 kinds of PDE-5 inhibitor class forbidden drugs carry out Quantitative Study, obtain quantitative test equation of linear regression.
Described health food is the food such as healthy medicated wine or health care Chinese medicine.
Compared with prior art, the present invention has following beneficial effect:
1. broad spectrum activity is strong: the present invention adopts PDE-5 inhibitor class forbidden drug in IDA-MS Screening analysis health food, utilize PDE-5 inhibitor class forbidden drug high-resolution Masterviews mass spectrometric data storehouse, fast qualitative Screening analysis bibliographical information 86 kinds of these type of materials, simultaneously by the database identify out novel violated western medicine composition of PDE-5 inhibitor do not reported, prove the detection broad spectrum activity of the method to forbidden drug in health food;
2. select 13 kinds of PDE-5 inhibitor class forbidden drugs such as Vardenafil hydrochloric acid, tadalafil, pseudo-Vardenafil to carry out Quantitative Study, standard regression curve linear is good, detectability is low, the detectability of 13 kinds of forbidden drugs at 1.2 ~ 3 μ g/L, the range of linearity 10 ~ 400 μ g/L;
3. matrix effect is little: the present invention adopts the m/z full scan type collection data of high resolution mass spectrum IDA-MS, and object utilizes and extracts Masterviews ion current chromatogram, according to the quantitative test of high-resolution firsts and seconds mass spectrometry;
4. preci-sion and accuracy is high: the present invention proves in the experiment of sample recovery of standard addition, and 13 kinds of PDE-5 inhibitor class forbidden drugs mix and are marked on 20,80, and the RSD of 3 kinds of concentration determinations such as 200 μ g/L is all within 5%;
5. good stability: the present invention proves in an experiment, after health care sample is placed 2 months, the accuracy absolute value of all samples is all less than 15%, shows long-time health food sample, does not affect this method and carries out preparation mensuration to sample concentration;
6.QuEChERS Dispersive solid phase extraction technology and ultrasound on extracting pre-treating method are simple, fast, accurately; The methods such as response surface design experimental design are utilized to optimize sample extraction condition, utilize recovery of standard addition as optimizing index, mix at 13 kinds of forbidden drugs and be marked on 20, in 80 μ g/L isoconcentration recovery of standard addition experiments, the recovery shows this pre-treating method validity 70.2 ~ 91.4%.
Accompanying drawing explanation
Fig. 1 is 13 kinds of PDE-5 inhibitor forbidden drug high-resolution firsts and seconds mass spectrograms; 1-1: Vardenafil; 1-2: pseudo-Vardenafil; 1-3: sulfo-Ai Dinafei; 1-4: hydroxyl Acctildenafil; 1-5:Genedenafil; 1-6: sulfo-silaenafil; 1-7: Acctildenafil; 1-8: person of outstanding talent is silaenafil not; 1-9: silaenafil; 1-10: hydroxyl person of outstanding talent not silaenafil; 1-11:Racxanthoabthrafil; 1-12: tadalafil; 1-13: amino tadalafil.
Fig. 2 is the chromatogram of 13 kinds of PDE-5 inhibitor forbidden drugs.
Fig. 3 is response surface design experimental design Optimized Extraction condition three-dimensional plot; A, C, E, I and K be QuEChERS respectively with four conditions: ACN:H2O of the ultrasonic pre-treatment that combines (, %v/v), MgSO4 & NaCl consumption (, mg), adsorbent C18 (, mg), ultrasonic time (, min) every two factors to that non-recycled rate of sulfo-Chinese mugwort ground three-dimension curved surface response diagram; B, D, F, H and L are that every two factors are to the three-dimension curved surface response diagram of the Genedenafil recovery.
Fig. 4 is the qualification of unknown PDE-5 inhibitor forbidden drug IDA-MS in health-care tonic wine; The MasterViewXICs examination qualification figure of A, a health-care tonic wine, B, demethyl silaenafil TOF-MS scheme, and C, demethyl silaenafil IDA-MS scheme, and D, Vardenafil IDA-MS scheme, and E, silaenafil IDA-MS scheme.
Embodiment
To make the present invention below in conjunction with Figure of description and specific embodiment and elaborating further, described embodiment, only for explaining the present invention, is not intended to limit scope of the present invention.The test method used in following embodiment if no special instructions, is conventional method; The material used, reagent etc. if no special instructions, are the reagent that can obtain from commercial channels and material.
Embodiment 1
The standard solution preparation of 1.13 kinds of PDE-5 inhibitor medicaments: PDE-5 inhibitor medicaments standard items respectively take 2.0mg, are placed in 10mL volumetric flask, by methanol constant volume to scale, are mixed with the standard reserving solution of 200 μ g/mL.Experimentally need to prepare 10 μ g/mL mixed standard solutions with methanol dilution, dilution preparation series standard working solution, 4 DEG C of preservations.
2.QuEChERS technology and ultrasound on extracting pre-treating method: utilize response surface design experimental design method, utilize Box-Behnken experimental design, 4 factors are respectively, ACN:H2O ratio (, %v/v), MgSO4 & NaCl consumption (, mg), adsorbent C18 (, mg), ultrasonic time (, min), quadratic regression equation model prediction assesses 13 kinds of PDE-5 inhibitor recovery of standard addition, since optimize four sample pre-treatments extraction factors.Box-Behnken experimental design gauge outfit is as following table:
Response surface design design factor and water-glass
Four factors are for 0 levels operation: 1mL tonic wine sample adds 15mL acetonitrile and water (70: 30) solution, 0.90g magnesium sulfate and 0.225g sodium chloride, 100mg adsorbent C18, abundant vortex 1min on micro-mixer, ultrasonic 15min, with the centrifugal 5min of 6000r/min rotating speed, constant volume in transfer supernatant to 25mL graduated tube, get 1mL solution and cross 0.45 μm of organic microporous Nylon filter membrane, treat that LC-Q-TOF-MS analyzes;
3. detecting instrument and analysis condition Japan Shimadzu Corporation LC-20AD liquid chromatograph and American AB sciex company's T riple
5600+ high-resolution mass spectrometer and LC-Q-TOF-MS,
tF1.6 image data software, the data analysis software such as Peakviews2.0, Multiquant3.0, Libraryview1.0
4.LC-Q-TOF-MS liquid phase chromatogram condition: water generation company of the U.S.
t3 (100mm × 3mm, 3 μm) chromatographic column, 40 DEG C of column temperatures, mobile phase A is 0.1% aqueous formic acid, Mobile phase B is acetonitrile, flow velocity 0.5mL/min, gradient elution: B phase increases to 30% by initial volume than 10%, 1min, 7min increases to 60%, 1min is down to 10%, retains 3min, sample size: 5 μ L.
5.LC-Q-TOF-MS Mass Spectrometry Conditions: ion gun: ESI and APCI multiple source; Positive ion scan mode; APCI source connects ABsciex company automatic correction system (CDS), every 10 sample automatic calibrations 1 time, APCI positive ion correcting fluid flow velocity 0.3mL/min, Curtaingas:40psi, ion gun gas1:50psi, ion gun gas2:50psi, ion source temperature: 500 DEG C, ion source voltage 5500V.One-level TOF-MS scans exact mass scope: 100 ~ 1000Da, data acquisition time 100ms, DP:100V, CE:10V; Secondary IDA-MS scans exact mass scope: 50 ~ 1000Da, DP:100V, CE:35 ± 15V; Highly sensitive pattern, data acquisition time 50ms, signal threshold value 100cps, IDA test every circle collection 6 secondary data, and dynamic background subtraction is deducted.
The firsts and seconds high resolution mass spectrum data (accompanying drawing 1) of 6.13 kinds of violated Western medicine standard items of PDE-5 inhibitor class, set up common PDE-5 inhibitor class Western medicine high resolution mass spectrum laboratory internal database.
7. the experimental data of response surface design experimental design Optimized Extraction, ACN:H
2o ratio (, %v/v), MgSO4 and NaCl consumption (, mg), adsorbent C18 consumption (, mg) and ultrasonic time (, 4 extraction conditionss such as min), wherein with sulfo-Ai Dinafei, gendenafil and sulfo-silaenafil recovery of standard addition for prediction index, gained response surface design experimental design data are in table 1, the three-dimensional plot optimizing 4 factors is shown in Fig. 3, and optimizing gained optimum extraction condition is ACN:H
2the percent by volume 60:40 (%v/v) of O, MgSO
4be respectively 1200mg and 300mg with the consumption of NaCl, the consumption of adsorbent C18 is 80mg, and ultrasonic time is 15min.
8. 13 kinds of PDE-5 inhibitor forbidden drug quantitative measurement researchs in health food: the mass spectrum quantitative basis (see table 2) obtaining object according to mass spectrophotometry, and the chromatogram of 13 kinds of objects (see Fig. 2), obtain quantitative test equation of linear regression, the range of linearity, related coefficient, detectability, the quantitative basis such as quantitative limit (see table 3), thus the content measuring 13 kinds of PDE-5 inhibitor forbidden drugs in health food.
Table 1 is response surface design experimental design Optimized Extraction condition data
Table 2 is the quantitative test mass spectrometric data of 13 kinds of PDE-5 inhibitor forbidden drugs
Table 3 is 13 kinds of the PDE-5 inhibitor forbidden drug ranges of linearity, detection limit and quantitative limit
Owing to can not contain 13 kinds of PDE-5 inhibitor forbidden drugs of quantitative test in tonic wine sample simultaneously, adopt recovery of standard addition methods of experiments accuracy, precision and stability.Tonic sample adds the PDE-5 inhibitor class medicine mixed standard solution of 60 μ g/L, and sample blank does not detect 13 kinds of PDE-5 inhibitor class medicines, and mark-on experimental result is in table 4.
Table 4 mark-on experimental result
Embodiment 2
Get 1mL tonic wine, add the mixed solution (volume ratio of acetonitrile and water is 7:3) of 15mL acetonitrile and water, 1g magnesium sulfate and 0.25g sodium chloride is added after mixing, abundant vortex 1min on micro-mixer, ultrasonic 10min, with the centrifugal 5min of 6000r/min rotating speed, constant volume in transfer supernatant to 25mL graduated tube, get 1mL solution and cross 0.45 μm of organic microporous Nylon filter membrane, detect for IDA-MS and analyze.The examination tables of data of PDE-5 inhibitor forbidden drug sees attached list 5, can analyze class forbidden drug (accompanying drawing 4) in health-care tonic wine by rapid screening, containing demethyl silaenafil forbidden drug composition in certain tonic wine sample according to high resolution mass spectrum data message.
Table 5 is 86 kinds of PDE-5 inhibitor forbidden drug Masterviews databases
Claims (3)
1. the non-targeted thing rapid screening detection method of the violated medicine of PDE-5 inhibitor class in health food, is characterized in that, comprise the steps:
S1. QuEChERS combine with technique ultrasound on extracting technology is adopted to carry out pre-treatment extraction to health food to be measured, extraction conditions is: the solution (the two volume ratio 6:4) adding 15mL acetonitrile and water in 1mL or 1g health food, 1.2g magnesium sulfate and 0.3g sodium chloride spreading agent, 80mg adsorbent C18, vortex, ultrasonic 10 ~ 15min, supernatant is got after centrifugal layering, supernatant constant volume is diluted, then the solution (volume ratio 6:4) that 1mL dilution adds 15mL acetonitrile and water is again got, vortex, ultrasonic, supernatant is got after centrifugal layering, supernatant constant volume dilutes, get 1mL again dilute after solution cross after organic system filter membrane as extraction sample liquid,
S2. get extraction sample liquid and carry out IDA-MS data acquisition: the condition of IDA-MS Screening analysis is: liquid phase separation condition is mobile phase A is 0.1% aqueous formic acid, Mobile phase B is acetonitrile, flow velocity 0.5mL/min, gradient elution: B phase increases to 30%, 7min by initial volume than 10%, 1min and increases to 60%, 1min is down to 10%, retain 3min, column temperature 40 DEG C, C18 chromatographic column; Gradient elution mode Mass Spectrometry Conditions: ESI and APCI multiple source; Positive ion scan mode; APCI source connects automatic correction system, and sample is ESI Ionization mode, Curtaingas:40psi, ion gun gas1:50psi, ion gun gas2:50psi, ion source temperature 500 DEG C, ion source voltage 5500V; One-level TOF-MS scans exact mass scope: 100 ~ 1000Da, data acquisition time 100ms, DP:100V, CE:10V; Secondary IDA-MS scans exact mass scope: 50 ~ 1000Da, DP:100V, CE:35 ± 15V; Highly sensitive pattern, data acquisition time 50ms, signal threshold value 100cps, IDA test every circle collection 6 secondary data, and dynamic background subtraction is deducted;
S3. the IDA-MS high resolution mass spectrum data analysis of sample, utilizes the process of PeakView data analysis software to obtain accurate molecular masses, isotopic molecule amount, molecular formula, the chromatographic retention of object, and accurate secondary fragment molecular weight; In conjunction with ChemSpider structural database, Qualitative Identification unknown PDE-5 inhibitor class western medicine composition.
2. detection method according to claim 1, it is characterized in that, select Vardenafil, pseudo-Vardenafil, sulfo-Ai Dinafei, hydroxyl Acctildenafil, Genedenafil, sulfo-silaenafil, Acctildenafil, person of outstanding talent not silaenafil, silaenafil, hydroxyl person of outstanding talent not silaenafil, Racxanthoabthrafil, tadalafil, amino tadalafil totally 13 kinds of PDE-5 inhibitor class forbidden drugs carry out Quantitative Study, obtain quantitative test equation of linear regression.
3. detection method according to claim 1, is characterized in that, described health food is healthy medicated wine or health care Chinese medicine.
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| CN108303486A (en) * | 2017-12-05 | 2018-07-20 | 广东出入境检验检疫局检验检疫技术中心 | The non-targeted object rapid detection method of forbidden drug in a kind of health food |
| CN109187798A (en) * | 2018-10-09 | 2019-01-11 | 山西省食品药品检验所(山西省药品包装材料监测中心) | Detect that non-, propoxyl group Chinese mugwort that non-, N- ethyl Tadalafei of ground of demethyl card rolling land and hydroxypropyl demethyl Tadalafei method |
| CN109406648A (en) * | 2018-09-28 | 2019-03-01 | 中国食品药品检定研究院 | Composition for illegal drug in testing product |
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| CN108303486A (en) * | 2017-12-05 | 2018-07-20 | 广东出入境检验检疫局检验检疫技术中心 | The non-targeted object rapid detection method of forbidden drug in a kind of health food |
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| CN109187798A (en) * | 2018-10-09 | 2019-01-11 | 山西省食品药品检验所(山西省药品包装材料监测中心) | Detect that non-, propoxyl group Chinese mugwort that non-, N- ethyl Tadalafei of ground of demethyl card rolling land and hydroxypropyl demethyl Tadalafei method |
| CN112394124A (en) * | 2020-11-05 | 2021-02-23 | 广州白云山医药集团股份有限公司白云山制药总厂 | Method for analyzing content of sildenafil, N-demethylsildenafil and N1, N4-dedimethyl sildenafil in plasma |
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Application publication date: 20160511 |