CN107515214A - Morphine, the quick determination method of codeine and detection kit in a kind of chafing dish food - Google Patents
Morphine, the quick determination method of codeine and detection kit in a kind of chafing dish food Download PDFInfo
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- CN107515214A CN107515214A CN201710623089.0A CN201710623089A CN107515214A CN 107515214 A CN107515214 A CN 107515214A CN 201710623089 A CN201710623089 A CN 201710623089A CN 107515214 A CN107515214 A CN 107515214A
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- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
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Abstract
The invention discloses morphine, the quick determination method of codeine and detection kit in a kind of chafing dish food.The present invention can be efficiently extracted morphine, the codeine in chafing dish food, directly be detected with morphine, codeine detection card using sample extracting solution and sodium acid carbonate processing chafing dish food.The detection method detection of the present invention is limited to 40 μ g/kg, Detection accuracy is 98%, specificity 97%, it can be very good the interference of related alkaloids and other matrix in exclusion chafing dish food, simple to operate, detection time is short, it is not necessary to Special Equipment, it is adapted to execute-in-place, suitable for superintendent office, the requirement of detection department, all kinds of mechanism field quick detections.
Description
Technical field
The present invention relates to field of food detection, more particularly, to the quick inspection of morphine, codeine in a kind of chafing dish food
Survey method and detection kit.
Background technology
Pappy shell is commonly called as opium shell, extracts the drying and ripening shell after juice for bloodroot opium poppy, includes kind more than 20
The most alkaloid of alkaloid, wherein content is respectively morphine, codeine, thebaine, papaverine, coscopin.Pappy shell has
Astringe the lung, puckery intestines, analgesic and other effects, there is certain medical value, as traditional Chinese medicine record in《Chinese Pharmacopoeia》.Pappy shell
In alkaloid can make one drowsiness and personality change, cause satisfied and floaty euphoria to a certain degree, people's notice, thinking can be caused
With the decline of memory performance, long-term consumption can cause insane, illusion occur, and breathing is resulted even in when serious and is stopped and dead
Die.With the addition of the food of pappy shell easily makes consumer's habituation, and long-term consumption person can be to it or psychological from body
Serious dependence is produced, causes serious toxicomania.
What State Council in 1987 enacted and enforced《Administration of narcotic drug method》Article 6, pappy shell is classified as management and control class fiber crops
Liquor-saturated medicine.National Drug Administration printed and distributed in 1998《Pappy shell manages temporary provisions》(state's pencil peace [1998] 127
Number), to the production of pappy shell, operation needed for the production prepared slices of Chinese crude drugs and Chinese patent drug and using special management is carried out, ensure medicine life
Production and medical treatment formula use, and prevent from flowing into illegal channels, to violator's foundation《Administration of narcotic drug method》Pertinent regulations are carried out
Punishment, it is in the case which constitutes a crime by judicial authority's prosecution for criminal responsibility shall be undertaken according to law.On December 12nd, 2008, the Ministry of Public Health promulgate《Can in food
The non-edible material from soybeans of the illegal addition of energy and the food additives kind list (first) easily abused》(food regulation does (2008) 3
Number), pappy shell is included into first batch of non-edible material from soybeans list.On January 3rd, 2011, the Ministry of Public Health promulgate on《May be illegal in food
The non-edible material from soybeans of addition and the food additives kind list easily abused》, pappy shell is classified as in food may illegal addition
Non- edible material from soybeans；Therefore opium poppy shell component is very necessary in detection food.
At present, in food opium poppy shell component detection, large-scale instrument detection mainly have liquid chromatography, gas chromatography,
Liquid Chromatography/Mass Spectrometry, gas chromatography mass spectrometry method etc.；Quick detection mainly has Raman spectroscopy, Near-Infrared Absorption Method, electrochemical process etc..Above method
Cumbersome, Check-Out Time length, is not suitable for the requirement of the field quick detections such as superintendent office, testing agency.Chafing dish is eaten at present
Morphine, the extracting method of codeine are complicated in product, and commercially available detection kit lacks supporting extracts reagent, and minority has supporting
Dilution, only sample is diluted, it is bad to solid and semisolid extraction effect, for the highly acid flavoring such as vinegar
It can not detect, it is impossible to meet the detection demand of the in the market flavoring various to matrix.
The content of the invention
It is an object of the invention to provide morphine, the quick determination method of codeine and detection reagent in a kind of chafing dish food
Box.
The technical solution used in the present invention is：
The quick determination method of morphine, codeine in a kind of chafing dish food, it is characterised in that comprise the following steps：
(1) chafing dish food is 1g by mass volume ratio with sample extracting solution：(3~6) mL is mixed, and is shaken 5~10 minutes, is obtained
Mixed liquor；
(2) it is (8~12) mL by the volume mass ratio of mixed liquor and sodium acid carbonate：1g addition sodium acid carbonates, shaking 5~
To reacting complete, 1~2 minute is stood, obtains prepare liquid within 10 minutes；
(3) prepare liquid water layer solution is drawn, is detected with morphine, codeine detection card.
As the preferred of the above method, in step (1), chafing dish food is 1g by mass volume ratio with sample extracting solution：(4
~5) mL is mixed.
It is 10mL by the volume mass of mixed liquor and sodium acid carbonate ratio in step (2) as the preferred of the above method：1g
Add sodium acid carbonate.
As the further preferred of the above method, sample extracting solution is 0.08~0.12mol/L hydrochloric acid solution.
As the preferred of the above method, sample extracting solution is 0.1mol/L hydrochloric acid solution.
As the preferred of the above method, sodium acid carbonate is powdered.
As the preferred of the above method, in step (2), reaction is complete to show as in solution that there is no bubble to emerge.
Morphine, the kit of codeine in a kind of quick detection chafing dish food, kit is interior to contain sample extracting solution, carbonic acid
Hydrogen sodium, morphine, codeine detection card.
As the preferred of mentioned reagent box, sample extracting solution is 0.08~0.12mol/L hydrochloric acid solution.
As the preferred of mentioned reagent box, sodium acid carbonate is powdered.
The beneficial effects of the invention are as follows：
The present invention can be efficiently extracted in chafing dish food using sample extracting solution and sodium acid carbonate processing chafing dish food
Morphine, codeine, directly detected with morphine, codeine detection card.The detection method detection of the present invention is limited to 40 μ g/kg,
Detection accuracy is 98%, specificity 97%, can be very good to exclude the dry of related alkaloids and other matrix in chafing dish food
Disturb, simple to operate, detection time is short, it is not necessary to Special Equipment, be adapted to execute-in-place, suitable for superintendent office, detection department, each
The requirement of class mechanism field quick detection.
Embodiment
Term " chafing dish food " of the present invention refers to the chafing dish based foods such as chafing dish bottom flavorings, flavoring, chafing dish soup bottom, due to chafing dish
It is no lack of matrix sourer or compared with alkali in food, often interference measurement, causes the detection of morphine, codeine to be forbidden.
With reference to specific embodiment, the present invention is further illustrated, but is not limited thereto.
Morphine used in the present invention, codeine detection card are purchased from Shenzhen Yi Rui bio tech ltd.
The quick detection kit of morphine, codeine in embodiment 1, chafing dish food
The quick detection kit of morphine, codeine in chafing dish food, kit is interior to contain sample extracting solution, sodium acid carbonate
Powder, morphine, codeine detection card；The sample extracting solution is 0.1mol/L hydrochloric acid solutions.
The quick determination method of morphine, codeine in embodiment 2, chafing dish food
The quick determination method of morphine, codeine, comprises the following steps in chafing dish food：
(1) 0.1mol/L hydrochloric acid solutions are prepared, as sample extracting solution；
(2) for Liquid chafing dish food, 1g samples are taken, add 4mL sample extracting solutions；Eaten for solid and semi-solid chafing dish
Product, 1g samples are taken, add 5mL sample extracting solutions；Shake 5~10 minutes and mix energetically；
(3) it is 10mL by the volume mass ratio of mixed liquor and sodium acid carbonate：1g adds sodium bicarbonate powder, shaking 5~10
Minute to emerge to there is no bubble, stands 1~2 minute, obtains prepare liquid；
(4) prepare liquid water layer solution is drawn, 4~5 is added dropwise and drips in the well that morphine, codeine detection block, according to
Coffee, codeine detection card specification operation and sentence read result：Detection card T lines do not develop the color, and judge to contain morphine in sample or can treat
Cause, judge not containing morphine and codeine in sample if detection card T line colour developings.
Points for attention：
1st, draw prepare liquid supernatant and avoid oil reservoir as far as possible；
2nd, when morphine, codeine detection card detection, develop the color 8~10 minutes and carry out result interpretation, result is invalid after 10 minutes；
The 3rd, if result display is positive, it is necessary to further carry out experimental analysis using the related official method of country in laboratory
With confirmation.
The sensitivity of embodiment 3, detection method
Morphine, each 5.0mg of codeine reference substance accurately are weighed, 5mL is settled to methanol dissolving, obtains the mono- mark deposits of 1mg/mL
Liquid；Solid, semisolid, Liquid chafing dish food 1g are weighed respectively in sample cell, it is each it is parallel take 11 parts, be separately added into various concentrations
Morphine, codeine list mark storing solution, obtain including morphine, the solid of codeine, semisolid and fluid sample；According to embodiment
2 method carries out extraction detection, show that the detection of detection method is limited to 40 μ g/kg.
Detection example 1
Known positive sample (being shown in Table 1) is tested using the method for embodiment 2.
The positive experimental result of table 1
| Numbering | Sample | Concentration | Quick detection result |
| 15982 | Spicy hot chafing dish soup bottom | The μ g/kg of morphine 654, the μ g/kg of codeine 552 | It is positive |
| 15983 | Chafing dish soup bottom | The μ g/kg of morphine 951, the μ g/kg of codeine 655 | It is positive |
| 14925 | Five-spice powder powder | The μ g/kg of morphine 92, the μ g/kg of codeine 102 | It is positive |
Detection example 2
50 batches of samples (20 batches of Liquid chafing dish food, 30 batches of solids, semi-solid chafing dish food) are collected altogether to implement the present invention
The method of example 2 is verified, while compared with confirming the result of method, confirmation uses food security provincial standard《DB
Pappy shell in 31/2010-2012 chafing dish foods, morphine, coscopin, the measure liquid chromatography-tandem matter of codeine and thebaine
Spectrometry》.
The screening results of table 2 and final confirmed results
The result of table 2 is shown：In addition to 1 lot sample product examine goes out false positive, remaining is consistent with confirmed results, the embodiment of the present invention 2
Method accuracy rate be 98%, specificity be 97%, false negative rate 0, false positive rate 3%, can effectively exclude chafing dish food
In other matrix interference.
Detection example 3
The food containing related alkaloids is detected using the method for embodiment 2, is as a result negative.It can be seen that when chafing dish food contains
Related alkaloids, this method will not be interfered.
Comparative example 1
The sample extracting solution that the present invention is substituted using purified water is tested, and other steps are the same as embodiment 2.As a result can detect
Morphine, codeine into chafing dish food, but detection limit is far above 40 μ g/kg.
Comparative example 2
With the contrast of food security provincial standard method.
Provincial standard method (DB 31/2010-2012) method pre-treatment is as follows：Chafing dish sauce, soup stock, flavored oils：Weigh
2g samples (being accurate to 0.01g) have in plug centrifuge tube in 50mL polytetrafluoroethylene (PTFE), add 150 μ L Isotopic Internal Standard working solutions, then
5mL water is added, shaking makes be uniformly dispersed (sauce class sample can add 10mL water if necessary), addition 15mL acetonitriles, vortex oscillation 1min,
The mixed-powder (or with suitable commercial goods replacement) of 6g anhydrous magnesium sulfates and 1.5g anhydrous sodium acetates is added, it is rapid to shake,
Vortex oscillation 1min, with 4000 revs/min of centrifugation 5min, take supernatant to be clean.
Solid kind toppings：Weigh 2g samples (being accurate to 0.01g) in 50mL polytetrafluoroethylene (PTFE) to have in plug centrifuge tube, add
150 μ L Isotopic Internal Standard working solutions, 5mL hydrochloric acid solutions are added, be ultrasonically treated 30 minutes, pH value is adjusted with sodium hydroxide solution
In neutrality, 15mL acetonitriles are added, vortex oscillation 1min, add the mixed-powder of 6g anhydrous magnesium sulfates and 1.5g anhydrous sodium acetates
(or with suitable commercial goods replacement), rapid shaking, vortex oscillation 1min, with 4000 revs/min of centrifugation 5min, take supernatant
It is to be clean.
Purification：50mg (± 5mg) PSA, 100mg (± 5mg) anhydrous magnesium sulfate is weighed, 100mg (± 5mg) C18 powder is put
Have in plug centrifuge tube (or with suitable commercial goods replacement) in 2mL polytetrafluoroethylene (PTFE), pipette 1.5mL supernatants so far centrifuge tube
In, vortex mixed 1min, with 10 000 revs/min of centrifugation 2min, supernatant is pipetted, 0.22 μm of membrane filtration, takes filtrate to be measured.
Pre-treatment is carried out to sample A3-39 according to provincial standard method (DB 31/2010-2012) method, it is real with the present invention
The method for applying the acquisition prepare liquid of example 2 is contrasted.
The upper liquid chromatography-tandem mass spectrometry detection of the prepare liquid that two methods obtain.
After provincial standard method (DB 31/2010-2012) pre-treatment, liquid chromatography-tandem mass spectrometry testing result is：
Coffee content：212 μ g/kg, codeine：50μg/kg；
The prepare liquid of the acquisition of the embodiment of the present invention 2, it is with liquid chromatography-tandem mass spectrometry testing result：Morphine content：
208 μ g/kg, codeine：48μg/kg；Using morphine, codeine detection card detection, T lines do not develop the color, are positive.
It these results suggest that：The sample pre-treatments of provincial standard method need to use assay balance, centrifuge, purification pipe,
The large-scale instruments such as liquid chromatograph-mass spectrometer, experimentation are cumbersome, it is necessary to time-consuming 1-2 days.And quick determination method of the present invention is not required to
Large-scale instrument is used, experimentation is simple, time-consuming short, can obtain qualitative results in 30 minutes, is adapted to execute-in-place.
Claims (10)
1. the quick determination method of morphine, codeine in a kind of chafing dish food, it is characterised in that comprise the following steps：
(1) chafing dish food is 1g by mass volume ratio with sample extracting solution：(3~6) mL is mixed, and is shaken 5~10 minutes, must be mixed
Liquid；
(2) it is (8~12) mL by the volume mass ratio of mixed liquor and sodium acid carbonate：1g adds sodium acid carbonate, shakes 5~10 minutes
It is complete to reaction, 1~2 minute is stood, obtains prepare liquid；
(3) prepare liquid water layer solution is drawn, is detected with morphine, codeine detection card.
2. quick determination method according to claim 1, it is characterised in that：In step (1), chafing dish food and sample extraction
Liquid is 1g by mass volume ratio：(4~5) mL is mixed.
3. quick determination method according to claim 1, it is characterised in that：In step (2), by mixed liquor and sodium acid carbonate
Volume mass ratio be 10mL：1g adds sodium acid carbonate.
4. quick determination method according to claim 1, it is characterised in that：Sample extracting solution is 0.08~0.12mol/L
Hydrochloric acid solution.
5. quick determination method according to claim 1, it is characterised in that：Sample extracting solution is that 0.1mol/L hydrochloric acid is molten
Liquid.
6. quick determination method according to claim 1, it is characterised in that：Sodium acid carbonate is powdered.
7. quick determination method according to claim 1, it is characterised in that：In step (2), reaction completely shows as molten
There is no bubble in liquid to emerge.
8. morphine, the kit of codeine in a kind of quick detection chafing dish food, it is characterised in that：Carried in kit containing sample
Take liquid, sodium acid carbonate, morphine, codeine detection card.
9. morphine, the kit of codeine in quick detection chafing dish food according to claim 8, it is characterised in that：Sample
Product extract solution is 0.08~0.12mol/L hydrochloric acid solution.
10. morphine, the kit of codeine in quick detection chafing dish food according to claim 8, it is characterised in that：Carbon
Sour hydrogen sodium is powdered.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108717089A (en) * | 2018-05-25 | 2018-10-30 | 三明出入境检验检疫局综合技术服务中心 | A kind of rapid detection method of papaverine, coscopin and thebaine |
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| CN1657938A (en) * | 2005-03-11 | 2005-08-24 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Colloidal gold immune test paper for investigating papaverine and its preparation method |
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| CN1657938A (en) * | 2005-03-11 | 2005-08-24 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Colloidal gold immune test paper for investigating papaverine and its preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108717089A (en) * | 2018-05-25 | 2018-10-30 | 三明出入境检验检疫局综合技术服务中心 | A kind of rapid detection method of papaverine, coscopin and thebaine |
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