CN107894485A - A kind of method of content of nitrosamines in detection food - Google Patents
A kind of method of content of nitrosamines in detection food Download PDFInfo
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- CN107894485A CN107894485A CN201711155449.5A CN201711155449A CN107894485A CN 107894485 A CN107894485 A CN 107894485A CN 201711155449 A CN201711155449 A CN 201711155449A CN 107894485 A CN107894485 A CN 107894485A
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- temperature
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- nitrosamines
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- dichloromethane
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Abstract
The invention discloses a kind of method for detecting content of nitrosamines in food, food to be measured is crushed, takes 15 25g to add in dichloromethane solution；After distillation, add 10 20mL acetone and carry out ultrasonic extraction, collect extract；Then to extract refrigerated centrifuge after, take 8 15mL supernatants to move in separatory funnel, with 3 8mL dichloromethane point extraction supernatants, collect dichloromethane layer liquid, be concentrated into 1mL, prepare liquid is made in concentrate after membrane filtration；Prepare liquid is determined by gas-chromatography thermal energy analyzer method for combined use, gas chromatographic column uses middle polarity chromatographic column, and carrier gas is helium；Gas-chromatography column temperature uses temperature programming.The principle of the invention is reliable, and experimental implementation is simple, make use of chromatogram and mass spectrographic high sensitivity, it is ensured that measurement accuracy and accuracy, disposably nitrosamine compound can be distinguished from numerous volatility organic components, greatly save analysis time and testing cost.
Description
Technical field
The present invention relates to technical field of food detection, specifically a kind of method for detecting content of nitrosamines in food.
Background technology
Nitrosamine is strong carcinogen, is one of most important chemical carcinogen, is one of four big food contaminants.Food,
All contain nitrosamine in cosmetics, beer, cigarette.In cured food is smoked, contain substantial amounts of nitrosamines material, some Digestives
System tumour, the incidence of disease such as the cancer of the esophagus are related to the nitrosamine quantity taken in meals.When smoked cured food and wine are taken in jointly,
Harm of the nitrosamine to health will be multiplied.
Organic component in food is numerous, and quick and precisely all nitrosamine compounds can be reflected currently without one kind
Other and tracking.Colorimetric method (AAS) detects, and this method sample treatment is cumbersome, and the interference of similar compound is big.Gas
Phase chromatograph-mass spectrometer coupling technology combines the determination molecular weight of the very effective separating capacity and mass spectrography of gas-chromatography and divided
The ability of minor structure, it is maximally efficient detection system generally acknowledged at present for analyzing and identifying complicated multicomponent organic mixture
One of system, but steam distillation is used, process complicated and time consumption length.
The content of the invention
It is an object of the invention to provide a kind of method for detecting content of nitrosamines in food, to solve above-mentioned background technology
The problem of middle proposition.
To achieve the above object, the present invention provides following technical scheme：
The method of content of nitrosamines, comprises the following steps in a kind of detection food：
1）Food to be measured is crushed, takes 15-25g to add in dichloromethane solution；After distillation, the progress of 10-20mL acetone is added
Ultrasonic extraction, collect extract；Then to extract refrigerated centrifuge after, take 8-15mL supernatants to move in separatory funnel, use
3-8mL dichloromethane point extraction supernatants, collect dichloromethane layer liquid, are concentrated into 1mL, concentrate is made after membrane filtration
Prepare liquid；
2）Prepare liquid is determined by gas-chromatography-thermal energy analyzer method for combined use, gas chromatographic column uses middle polarity chromatographic column,
Carrier gas is helium；Gas-chromatography column temperature uses temperature programming.
As the further scheme of the present invention：Step 1）In, dichloromethane solution is that the volume ratio of dichloromethane and water is
2-5:5-15。
As the further scheme of the present invention：Step 1）In, the temperature 50 C of ultrasonic extraction, ultrasonic power 400-
1000W, ultrasonic time 15min.
As the further scheme of the present invention：Step 1）In, concentration process is revolved after using anhydrous sodium sulfate dewatering and filtering
Turn evaporation.
As the further scheme of the present invention：Rotating evaporation temperature is 50 DEG C.
As the further scheme of the present invention：Step 1）In, filter membrane uses 0.20-0.25 μm of miillpore filter.
As the further scheme of the present invention：Step 2）In, gas chromatographic detection condition is：230 DEG C of injector temperature, enters
The μ L of sample amount 2, chromatographic column use DB624 chromatographic columns, and gas-chromatography column temperature uses temperature programming：60 DEG C of holding 5- of initial temperature
6min, 20 DEG C/min temperature programmings to 120 DEG C, keep 3-6min, 3 DEG C/min temperature programmings to 140 DEG C, keep 2-4min, 10
DEG C/min temperature programmings to 250 DEG C, keep 2-5min.
As the further scheme of the present invention：Step 2）In, the condition of thermal energy analyzer is：250 DEG C of interface temperature, cracking
550 DEG C of device temperature, ozone flow 12mL/min, -20 DEG C of chilling temperature, voltage 780V.
Compared with prior art, the beneficial effects of the invention are as follows：
The principle of the invention is reliable, and experimental implementation is simple, make use of chromatogram and mass spectrographic high sensitivity, it is ensured that measurement accuracy and standard
Degree, disposably can distinguish nitrosamine compound from numerous volatility organic components, can be directly to limited, few
Several related nitrosamine compounds is carried out qualitative and quantified, and greatlys save analysis time and testing cost.The present invention is applied to food
Product it is actually detected, technical method can be provided for the detection of food nitrite nitramine and control of product quality and supported.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of method for detecting content of nitrosamines in food, comprise the following steps：
1）Food to be measured is crushed, takes 15g to add in dichloromethane solution；Dichloromethane solution is the volume of dichloromethane and water
Than for 2:5.After distillation, add 10mL acetone and carry out ultrasonic extraction, collect extract；The temperature 50 C of ultrasonic extraction, ultrasound
Power is 400W, ultrasonic time 15min.Then to extract refrigerated centrifuge after, take 8mL supernatants to move in separatory funnel,
With 3mL dichloromethane point extraction supernatants, dichloromethane layer liquid is collected, is concentrated into 1mL, concentrate is through 0.20 μm of miillpore filter
Prepare liquid is made after filtering；Concentration process is to use rotary evaporation after anhydrous sodium sulfate dewatering and filtering.Rotating evaporation temperature is 50
℃。
2）Prepare liquid is determined by gas-chromatography-thermal energy analyzer method for combined use, gas chromatographic column uses middle polarity color
Post is composed, carrier gas is helium；Gas-chromatography column temperature uses temperature programming.Gas chromatographic detection condition is：230 DEG C of injector temperature,
The μ L of sample size 2, chromatographic column use DB624 chromatographic columns, and gas-chromatography column temperature uses temperature programming：60 DEG C of holdings of initial temperature
5min, 20 DEG C/min temperature programmings to 120 DEG C, keep 3min, 3 DEG C/min temperature programmings to 140 DEG C, keep 2min, 10 DEG C/
Min temperature programmings keep 2min to 250 DEG C.The condition of thermal energy analyzer is：250 DEG C of interface temperature, 550 DEG C of cracker temperature,
Ozone flow 12mL/min, -20 DEG C of chilling temperature, voltage 780V.
Embodiment 2
In the embodiment of the present invention, a kind of method for detecting content of nitrosamines in food, comprise the following steps：
1）Food to be measured is crushed, takes 25g to add in dichloromethane solution；Dichloromethane solution is the volume of dichloromethane and water
Than for 5:15.After distillation, add 20mL acetone and carry out ultrasonic extraction, collect extract；The temperature 50 C of ultrasonic extraction, ultrasound
Power is 1000W, ultrasonic time 15min.Then to extract refrigerated centrifuge after, take 15mL supernatants to move to separatory funnel
In, with 8mL dichloromethane point extraction supernatants, dichloromethane layer liquid is collected, is concentrated into 1mL, concentrate is through 0.25 μm of micropore
Prepare liquid is made after membrane filtration；Concentration process is to use rotary evaporation after anhydrous sodium sulfate dewatering and filtering.Rotating evaporation temperature
For 50 DEG C.
2）Prepare liquid is determined by gas-chromatography-thermal energy analyzer method for combined use, gas chromatographic column uses middle polarity color
Post is composed, carrier gas is helium；Gas-chromatography column temperature uses temperature programming.Gas chromatographic detection condition is：230 DEG C of injector temperature,
The μ L of sample size 2, chromatographic column use DB624 chromatographic columns, and gas-chromatography column temperature uses temperature programming：60 DEG C of holdings of initial temperature
6min, 20 DEG C/min temperature programmings to 120 DEG C, keep 6min, 3 DEG C/min temperature programmings to 140 DEG C, keep 4min, 10 DEG C/
Min temperature programmings keep 5min to 250 DEG C.The condition of thermal energy analyzer is：250 DEG C of interface temperature, 550 DEG C of cracker temperature,
Ozone flow 12mL/min, -20 DEG C of chilling temperature, voltage 780V.
Embodiment 3
In the embodiment of the present invention, a kind of method for detecting content of nitrosamines in food, comprise the following steps：
1）Food to be measured is crushed, takes 20g to add in dichloromethane solution；Dichloromethane solution is the volume of dichloromethane and water
Than for 3:10.After distillation, add 15mL acetone and carry out ultrasonic extraction, collect extract；The temperature 50 C of ultrasonic extraction, ultrasound
Power is 600W, ultrasonic time 15min.Then to extract refrigerated centrifuge after, take 12mL supernatants to move in separatory funnel,
With 5mL dichloromethane point extraction supernatants, dichloromethane layer liquid is collected, is concentrated into 1mL, concentrate is through 0.22 μm of miillpore filter
Prepare liquid is made after filtering；Concentration process is to use rotary evaporation after anhydrous sodium sulfate dewatering and filtering.Rotating evaporation temperature is 50
℃。
2）Prepare liquid is determined by gas-chromatography-thermal energy analyzer method for combined use, gas chromatographic column uses middle polarity color
Post is composed, carrier gas is helium；Gas-chromatography column temperature uses temperature programming.Gas chromatographic detection condition is：230 DEG C of injector temperature,
The μ L of sample size 2, chromatographic column use DB624 chromatographic columns, and gas-chromatography column temperature uses temperature programming：60 DEG C of holdings of initial temperature
5min, 20 DEG C/min temperature programmings to 120 DEG C, keep 5min, 3 DEG C/min temperature programmings to 140 DEG C, keep 3min, 10 DEG C/
Min temperature programmings keep 2min to 250 DEG C.The condition of thermal energy analyzer is：250 DEG C of interface temperature, 550 DEG C of cracker temperature,
Ozone flow 12mL/min, -20 DEG C of chilling temperature, voltage 780V.
Using volatilize N- nitrosamine and interior target peak area ratio as ordinate, with the concentration (ng/mL) of various nitrosamine
Standard curve is drawn for abscissa.According to the curvilinear equation drawn, method detection is limited to 12.5-25 μ g/kg.The present invention is to 8 parts
Totally 18 parts of samples are analyzed for cured meat product, 10 portions of pickles, and analysis result shows, this method can be effectively to nitrous therein
Amines carries out full inspection survey, has good reappearance.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (8)
- A kind of 1. method for detecting content of nitrosamines in food, it is characterised in that comprise the following steps：1）Food to be measured is crushed, takes 15-25g to add in dichloromethane solution；After distillation, the progress of 10-20mL acetone is added Ultrasonic extraction, collect extract；Then to extract refrigerated centrifuge after, take 8-15mL supernatants to move in separatory funnel, use 3-8mL dichloromethane point extraction supernatants, collect dichloromethane layer liquid, are concentrated into 1mL, concentrate is made after membrane filtration Prepare liquid；2）Prepare liquid is determined by gas-chromatography-thermal energy analyzer method for combined use, gas chromatographic column uses middle polarity chromatographic column, Carrier gas is helium；Gas-chromatography column temperature uses temperature programming.
- 2. the method for content of nitrosamines in detection food according to claim 1, it is characterised in that step 1）In, dichloro Dichloromethane is that the volume ratio of dichloromethane and water is 2-5:5-15.
- 3. the method for content of nitrosamines in detection food according to claim 1, it is characterised in that step 1）In, ultrasound The temperature 50 C of extraction, ultrasonic power 400-1000W, ultrasonic time 15min.
- 4. the method for content of nitrosamines in detection food according to claim 1, it is characterised in that step 1）In, concentration Process is to use rotary evaporation after anhydrous sodium sulfate dewatering and filtering.
- 5. the method for content of nitrosamines in detection food according to claim 4, it is characterised in that rotating evaporation temperature is 50℃。
- 6. the method for content of nitrosamines in detection food according to claim 1, it is characterised in that step 1）In, filter membrane Using 0.20-0.25 μm of miillpore filter.
- 7. the method for content of nitrosamines in detection food according to claim 1, it is characterised in that step 2）In, gas phase Chromatographic test strip part is：230 DEG C of injector temperature, the μ L of sample size 2, chromatographic column use DB624 chromatographic columns, and gas-chromatography column temperature is adopted Use temperature programming：60 DEG C of initial temperature holding 5-6min, 20 DEG C/min temperature programmings keep 3-6min to 120 DEG C, 3 DEG C/min Temperature programming keeps 2-4min to 140 DEG C, and 10 DEG C/min temperature programmings keep 2-5min to 250 DEG C.
- 8. the method for content of nitrosamines in detection food according to claim 1, it is characterised in that step 2）In, heat energy The condition of analyzer is：250 DEG C of interface temperature, 550 DEG C of cracker temperature, ozone flow 12mL/min, -20 DEG C of chilling temperature, Voltage 780V.
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| US3996009A (en) * | 1975-09-17 | 1976-12-07 | Thermo Electron Corporation | Specific compound detection system |
| RU2241219C1 (en) * | 2003-05-20 | 2004-11-27 | Государственное образовательное учреждение высшего профессионального образования Санкт-Петербургская государственная медицинская академия им. И.И. Мечникова | Method of determining toxicity of 1-nitrosamines in foods |
| CN104062377A (en) * | 2014-07-04 | 2014-09-24 | 湖南科技大学 | Total-detection method of volatile N-nitrosamine compounds in foods |
| US20150121993A1 (en) * | 2013-11-05 | 2015-05-07 | King Abdulaziz City For Science And Technology | Dispersive liquid-liquid microextraction method of detecting n-nitrosoamines |
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| CN106324157A (en) * | 2016-10-27 | 2017-01-11 | 安徽易康达光电科技有限公司 | Method for quickly detecting volatile N-nitrosamine in cosmetics |
-
2017
- 2017-11-20 CN CN201711155449.5A patent/CN107894485A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US3996009A (en) * | 1975-09-17 | 1976-12-07 | Thermo Electron Corporation | Specific compound detection system |
| RU2241219C1 (en) * | 2003-05-20 | 2004-11-27 | Государственное образовательное учреждение высшего профессионального образования Санкт-Петербургская государственная медицинская академия им. И.И. Мечникова | Method of determining toxicity of 1-nitrosamines in foods |
| US20150121993A1 (en) * | 2013-11-05 | 2015-05-07 | King Abdulaziz City For Science And Technology | Dispersive liquid-liquid microextraction method of detecting n-nitrosoamines |
| CN104062377A (en) * | 2014-07-04 | 2014-09-24 | 湖南科技大学 | Total-detection method of volatile N-nitrosamine compounds in foods |
| CN104614470A (en) * | 2014-10-31 | 2015-05-13 | 傅武胜 | Detection method for volatile nitrosamine in fish and meat products and pretreatment device |
| CN106324157A (en) * | 2016-10-27 | 2017-01-11 | 安徽易康达光电科技有限公司 | Method for quickly detecting volatile N-nitrosamine in cosmetics |
Non-Patent Citations (2)
| Title |
|---|
| SEO JUNG-EUN 等: "Determination of Seven N-nitrosamines in Agricultural Food Matrices Using GC-PCI-MS/MS", 《FOOD ANALYTICAL METHODS》 * |
| 张红 等: "气相色谱-热能分析仪测定水产品中N-亚硝胺", 《食品研究与开发》 * |
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Application publication date: 20180410 |