CN106124642A - A kind of green tea determination of acrylamide and application - Google Patents
A kind of green tea determination of acrylamide and application Download PDFInfo
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- CN106124642A CN106124642A CN201610319641.2A CN201610319641A CN106124642A CN 106124642 A CN106124642 A CN 106124642A CN 201610319641 A CN201610319641 A CN 201610319641A CN 106124642 A CN106124642 A CN 106124642A
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- acrylamide
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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 relates to technical field of analysis and detection, affect the Detection results problem of method for solution mensuration Acrylamide in Foods content at present because of different food products substrate, the present invention proposes a kind of green tea determination of acrylamide and application, with13C3Acrylamide is internal standard, use more options reaction monitoring pattern, proved by methodology, build green tea acrylamide quantitative analysis method based on HPLC MS/MS, the detection method accuracy of the present invention, repeatability, stability are preferable, are suitable to the actually detected of acrylamide in green tea.
Description
Technical field
The present invention relates to technical field of analysis and detection, relate in particular to a kind of green tea determination of acrylamide and answer
With.
Background technology
Acrylamide (Acrylamide), chemical molecular formula CH2CHCONH2, it is the water white transparency lamellar knot of a kind of readily soluble water
Crystalline substance, common are machine synthesis material as one, is industrially widely used.IARC (IRAC)
Acrylamide is classified as IIA class carcinogen；WHO thinks that " carcinogenicity risk is more than 10-5Standard be 0.5ug/L "；From 2002
Year, Sweden scientist found that starch food products i.e. causes after producing substantial amounts of acrylamide in high temperature working processes entirely first
Ball extensive concern.
China is Folium Camelliae sinensis big country of the world, and tea place area, tea yield occupy the first in the world.Folium Camelliae sinensis endoplasm composition enriches, and adds
Work operation is various, and tea kind is many, there are some researches show, in tea making process, Folium Camelliae sinensis endoplasm becomes branch that complicated chemical change occurs, from
And producing the potential hazard things such as acrylamide, Tea Processing process safety has become the new focus that field of food safety is paid close attention to.Mesh
Before, in the world use HPLC-MS/MS methods to measure Acrylamide in Foods content more, the method is simple to operate, sensitivity relatively
Height, but different food products substrate can affect the Detection results of method.
Summary of the invention
The Detection results problem of method is affected because of different food products substrate for solution mensuration Acrylamide in Foods content at present,
The present invention proposes a kind of green tea determination of acrylamide and application, and detection method accuracy, repeatability, stability are preferable,
Be suitable to the actually detected of acrylamide in green tea.
The present invention is achieved by the following technical solutions: a kind of green tea determination of acrylamide is:
(1) sample pre-treatments:
Weigh the green tea sample after pulverizing and be sequentially added into formic acid, isotope labelling acrylamide standard solution, mixing,
30-90 DEG C of water-bath the 10-60min that vibrates；Then it is sequentially added into acetonitrile, magnesium sulfate, sodium chloride, seals vibration, centrifugal；Take supernatant
Liquid, under water-bath, nitrogen dries up, and filters, obtains pretreatment sample；
Described isotope labelling acrylamide standard solution is13C3-acrylamide is dissolved in concentration of volume percent
0.1% formic acid prepares,13C3The concentration of-acrylamide is 30-70ng/mL.
Green tea powder, formic acid, the mass volume ratio of isotope labelling acrylamide standard solution are 1g: 7-11mL: 0.8-
1.2mL。
Green tea powder, acetonitrile, magnesium sulfate, the mass volume ratio of sodium chloride are 1g: 9-11mL: 3-5g: 0.5-1.5g.
As preferably, it is centrifuged 4-10min by 5000-12000rpm/min, takes supernatant, nitrogen under 30-90 DEG C of water-bath
Air-blowing is done, through 0.45 μm filtering with microporous membrane.
(2) purify: use solid-phase extraction column that pretreatment sample is carried out purified treatment, obtain testing sample；
Described purification method is: after solid-phase extraction column is carried out pretreatment, the pretreatment sample that step (1) obtains is entered
Row loading, collects permeate, crosses film, obtains testing sample.
(3) use high performance liquid chromatography tandem mass spectrum method that testing sample is detected, calculate acryloyl by internal standard method
Amine content.Respectively sample and serial standards are injected HPLC-MS/MS system, record acrylamide and13C3-acrylamide peak
Area, with acrylamide and13C3The concentration of-acrylamide ratio is for abscissa, and peak area ratio is vertical coordinate mapping, draws acryloyl
Amine standard curve.Thus calculate the content of acrylamide in sample.As preferably, each process carries out three times and repeats, and takes it and puts down
Average is analyzed.
Chromatograph test condition is: flowing includes water, mixed liquor and the flowing phase of acetonitrile that volumetric concentration is 99.9% mutually
Volumetric concentration is the formic acid of 0.1%；Flow velocity is 200 μ L/min；Sampling volume 10 μ L；Column temperature 34-36 DEG C, Qi Zhongshui, acetonitrile
In mixed liquor, water is 99: 1 with the volume ratio of acetonitrile.
Mass Spectrometry Conditions: Ionization mode is ESI ion source；Scan mode is for just to ionize；Detection mode is polyion reaction
Monitoring, collision energy is 8eV, collision induced dissociation voltage: 50V.
Ion source condition: be dried temperature: 325C；Dry gas stream speed: 5L/min；Atomization gas pressure: 45psi；Sheath temperature
Degree: 350 DEG C；Sheath gas velocity: 11L/min；Capillary voltage: 3000V, wherein:
The present invention is directed to green tea medium characteristics, optimize sample-pretreating method, with13C3-acrylamide is internal standard, and employing is many
Selective reaction monitoring (MRM) pattern, is proved by methodology, builds green tea acrylamide quantitative analysis based on HPLC-MS/MS
Method, is applied in tea district tea sample analysis method according to this analysis method, 10 of Chan Cha district main to China simultaneously
Green tea sample has carried out Determination of acrylamide.
Compared with prior art, the invention has the beneficial effects as follows: the detection method accuracy of the present invention, repeatability, stable
Property preferable, be suitable to the actually detected of acrylamide in green tea.
Accompanying drawing explanation
Fig. 1 is embodiment acrylamide canonical plotting；
Fig. 2 is in the mixed mark of embodiment13C3-acrylamide, the MRM mass spectrum of acrylamide；
Fig. 3 is embodiment green tea sample13C3-acrylamide, the MRM mass spectrum of acrylamide.
Specific implementation method
Below by embodiment, the present invention is described in further details, raw materials used the most commercially available or with often in embodiment
Prepared by rule method.
Acrylamide standard substance in embodiment, purity ＞ 95%, (ChemService company, the U.S.)；13C3-acrylamide
Standard substance, purity ＞ 99%, (ChemService company, the U.S.)；Methanol, acetonitrile (chromatographically pure), formic acid (chromatographically pure), just oneself
Alkane, magnesium sulfate (MgSO4), sodium chloride (NaCl) be purchased from Chemical Reagent Co., Ltd., Sinopharm Group.Accurately weigh 0.1g propylene
Amide standard substance are dissolved in 100mL volumetric flask, dissolve with ultra-pure water and are diluted to scale, in-20 DEG C of Refrigerator stores as deposit
Solution, compound concentration is 1,5,10,50 and the acrylamide standard solution of 100ng/mL,13C3-acrylamide is internal standard, concentration
For 50ng/mL.
Agilent 6460 Triple Quad LC-MS triplex tandem quadrupole rod LC-MS instrument in embodiment,
Agilent Zorbax SB C18Post (150mm × 2.1mm, 3.5 μm)；SPE solid-phase extraction column Cleanert PCX (60mg, sky
Tianjin Beaune Ai Jieer company limited), utilize Mass hunter liquid matter workstation software (Agilent company, the U.S.) to gather relevant
Data.
Embodiment 1
(1) weigh 1g pulverize after green tea sample in 50mL centrifuge tube, being sequentially added into 9mL volumetric concentration is 0.1% first
Acid, 1mL50ng/mL internal standard liquid (13C3-acrylamide is dissolved in 0.1% formic acid), mixing, water-bath vibration at 30 DEG C
20min；It is subsequently adding 10mL acetonitrile, 4g magnesium sulfate, 1g sodium chloride, seals the 1min that acutely vibrates rapidly, be centrifuged in 5000r/min
10min, takes supernatant 8ml, and under 40 DEG C of water-baths, nitrogen dries up；Take 1ml ultra-pure water and dissolve the residue on test tube wall, through 0.45
The filtering with microporous membrane of μm.
(2) pretreatment sample that step (1) obtains is carried out loading, after solid-phase extraction column is carried out pretreatment, collect thoroughly
Cross liquid, through 0.22 μm membrane filtration, to be measured.
(3) detection is analyzed by HPLC-MS/MS
Chromatographic condition: flowing is water-acetonitrile (99: 1, V/V) mixed liquor mutually, and volumetric concentration is 99,9%, and volumetric concentration is
The formic acid of 0.1%；Flow velocity is 200 μ L/min；Sampling volume 10 μ L；Column temperature 35C.
Mass Spectrometry Conditions: Ionization mode: ESI ion source；Scan mode: just ionize；Scanning ion pair: acrylamide (m/z
72-55),13C3-acrylamide (m/z 75.2-58.1).Detection mode: polyion reaction monitoring (MRM), collision energy: 8eV,
Collision induced dissociation voltage: 50V.Ion source condition: be dried temperature: 325C；Dry gas stream speed: 5L/min；Atomization gas pressure:
45psi；Sheath temperature: 350 DEG C；Sheath gas velocity: 11L/min；Capillary voltage: 3000V.
Respectively sample and serial standards are injected HPLC-MS/MS system, record acrylamide and13C3-acrylamide peak
Area, with acrylamide and13C3The concentration of-acrylamide ratio is for abscissa, and peak area ratio is vertical coordinate mapping, draws acryloyl
Amine standard curve.Thus calculate the content of acrylamide in sample.Each process carries out three times and repeats, and takes its meansigma methods and carries out point
Analysis, data are usedRepresent.
Embodiment 2
(1) weigh 1g pulverize after green tea sample in 50mL centrifuge tube, being sequentially added into 7mL volumetric concentration is 0.1% first
Acid, 0.8mL30ng/mL internal standard liquid (13C3-acrylamide is dissolved in 0.1% formic acid), mixing, water-bath vibration at 90 DEG C
10min；Be subsequently adding 9mL acetonitrile, 5g magnesium sulfate, 0.5g sodium chloride, seal the 1min that acutely vibrates rapidly, in 7000r/min from
Heart 7min, takes supernatant 8ml, and under 90 DEG C of water-baths, nitrogen dries up；Take 1ml ultra-pure water and dissolve the residue on test tube wall, warp
The filtering with microporous membrane of 0.45 μm；
(2) pretreatment sample that step (1) obtains is carried out loading, after solid-phase extraction column is carried out pretreatment, collect thoroughly
Cross liquid, through 0.22 μm membrane filtration, to be measured.
(3) detection is analyzed by HPLC-MS/MS
Chromatographic condition: flowing is water-acetonitrile (99: 1, V/V) mutually, and mixed liquor, volumetric concentration is 99,9%, and volumetric concentration is
The formic acid of 0.1%；Flow velocity is 200 μ L/min；Sampling volume 10 μ L；Column temperature 34C.
Mass Spectrometry Conditions: Ionization mode: ESI ion source；Scan mode: just ionize；Scanning ion pair: acrylamide (m/z
72-55),13C3-acrylamide (m/z 75.2-58.1).Detection mode: polyion reaction monitoring (MRM), collision energy: 8eV,
Collision induced dissociation voltage: 50V.Ion source condition: be dried temperature: 325C；Dry gas stream speed: 5L/min；Atomization gas pressure:
45psi；Sheath temperature: 350 DEG C；Sheath gas velocity: 11L/min；Capillary voltage: 3000V.
Respectively sample and serial standards are injected HPLC-MS/MS system, record acrylamide and13C3-acrylamide peak
Area, with acrylamide and13C3The concentration of-acrylamide ratio is for abscissa, and peak area ratio is vertical coordinate mapping, draws acryloyl
Amine standard curve.Thus calculate the content of acrylamide in sample.Each process carries out three times and repeats, and takes its meansigma methods and carries out point
Analysis, data are usedRepresent.
Embodiment 3
(1) weigh 1g pulverize after green tea sample in 50mL centrifuge tube, being sequentially added into 11mL volumetric concentration is 0.1% first
Acid, 1.2mL70ng/mL internal standard liquid (13C3-acrylamide is dissolved in 0.1% formic acid), mixing, water-bath vibration at 50 DEG C
60min；It is subsequently adding 11mL acetonitrile, 3g magnesium sulfate, 1.5g sodium chloride, seals the 1min that acutely vibrates rapidly, in 12000r/min
Centrifugal 4min, takes supernatant 8ml, and under 50 DEG C of water-baths, nitrogen dries up；Take 1ml ultra-pure water and dissolve the residue on test tube wall, warp
The filtering with microporous membrane of 0.45 μm.
(2) pretreatment sample that step (1) obtains is carried out loading, after solid-phase extraction column is carried out pretreatment, collect thoroughly
Cross liquid, through 0.22 μm membrane filtration, to be measured.
(3) detection is analyzed by HPLC-MS/MS
Chromatographic condition: flowing is water-acetonitrile (99: 1, V/V) mixed liquor mutually, and volumetric concentration is 99,9%, and volumetric concentration is
The formic acid of 0.1%；Flow velocity is 200 μ L/min；Sampling volume 10 μ L；Column temperature 36C.
Mass Spectrometry Conditions: Ionization mode: ESI ion source；Scan mode: just ionize；Scanning ion pair: acrylamide (m/z
72-55),13C3-acrylamide (m/z 75.2-58.1).Detection mode: polyion reaction monitoring (MRM), collision energy: 8eV,
Collision induced dissociation voltage: 50V.Ion source condition: be dried temperature: 325C；Dry gas stream speed: 5L/min；Atomization gas pressure:
45psi；Sheath temperature: 350 DEG C；Sheath gas velocity: 11L/min；Capillary voltage: 3000V.
Respectively sample and serial standards are injected HPLC-MS/MS system, record acrylamide and13C3-acrylamide peak
Area, with acrylamide and13C3The concentration of-acrylamide ratio is for abscissa, and peak area ratio is vertical coordinate mapping, draws acryloyl
Amine standard curve.Thus calculate the content of acrylamide in sample.Each process carries out three times and repeats, and takes its meansigma methods and carries out point
Analysis, data are usedRepresent.
Embodiment 1～3 with series standard solution sample introduction, record acrylamide and13C3-acrylamide peak area, with propylene
Amide and13C3The corresponding corresponding peak area ratio of-acrylamide concentration carries out linear regression analysis, obtains the standard of acrylamide
Curve, regression equation is: y=1.1219 × x+0.02750, R2=0.9999, acrylamide content is in 1～100ng/mL scope
Present good linear relationship, meet quantitative requirement, as shown in Figure 1.Acrylamide mixes the MRM mass spectrum of mark and green tea sample to be seen
Fig. 2, Fig. 3, as seen from the figure, in standard specimen and sample, acrylamide standard substance retention time is 2.83min, internal standard13C3-propylene
Amide retention time is 2.83min, and retention time is consistent.
Application examples 1: repeatability is tested
Precision weighs 5 parts of samples, quality respectively: 1.0012,1.0031,1.0055,1.0016,1.0013g, pass through sample
Product pre-treatment and sample introduction analysis, calculate the acrylamide content of 5 parts of samples be respectively 26.90,25.67,26.89,
28.72,25.07ng/g, meansigma methods is 26.65ng/g, RSD=5.26% (n=5), shows that the method repeatability is preferable.
Application examples 2: matrix effect and the response rate
(1) recovery test
In green tea sample, add the acrylamide standard solution of variable concentrations, arrange basic, normal, high three add scalar be 2,
50,80ng/mL, extracts according to fixed sample-pretreating method, uses HPLC-MS/MS method to measure acrylamide and contains
Amount, each sample replication 3 times, calculate recovery of standard addition, the results are shown in Table 1.It follows that basic, normal, high 3 concentration levels
Under recovery of standard addition be all higher than 70%, relative standard deviation is respectively less than 6.0%.
(2) matrix effect test
Matched group 1 is set to using methanol as the mixed mark of solvent preparation；Matched group 2, for taking green tea sample, measures its acryloyl
Amine content；Experimental group is for taking green tea sample, and the acrylamide standard solution post analysis adding variable concentrations measures, and arranges acryloyl
Amine standard substance final concentration is respectively 2,50,80ng/mL,13C3-acrylamide internal standard concentration is 20ng/mL.Repeat with each sample
Measure 3 times, calculate matrix effect, the results are shown in Table 1.It follows that the recovery of standard addition under basic, normal, high 3 concentration levels is the biggest
In 84%, relative standard deviation is respectively less than 6.0%, has feature accurate, reliable, is suitable to the actual inspection of acrylamide in Folium Camelliae sinensis
Survey.
Table 1 response rate and matrix effect
Application examples 3:LOD and LOQ
The detection limit basis of HPLC-MS/MS method determines signal to noise ratio, with 3 times of signal-to-noise ratio computation to the mensuration of bare substrate
Qualitative detection limit, 10 times of signal-to-noise ratio computation detection by quantitative limits, parallel assay 3 times, average, draw the qualitative detection of the method
Limit (LOD) is 1.0ng/g, and quantitative detection limit (LOQ) is 10.0ng/g.
Application examples 4: tea district tea sample is analyzed
The green tea in Chan Cha district main to the whole nation is sampled detection, finds generally to contain acrylamide in green tea.Table 2 shows
The testing result of acrylamide in ten kinds of green tea samples, in sample, acrylamide content is 5.17～26.65ng/g, averagely contains
Amount is 10.86ng/g, and wherein sample 5, sample 6, sample 8 exceed average level, and each green tea Differences is bigger.Sample 8 is
Take from the green tea sample in Jiangsu, its acrylamide detection value the most higher (26.65ng/g), high nearer than sample 4 (1.53ng/g)
17 times, there is the biggest difference in the content of acrylamide, reason may be caused by Overheating Treatment during Green Tea Processing.
Acrylamide content in 20 kinds of green tea samples of table
From the point of view of measurement result, generally there is acrylamide in green tea, individual plants content is higher.For guaranteeing tea quality
Safety, must strengthen the monitoring to acrylamide Conduce Disciplinarian, acrylamide minimizing skill during research Green Tea Processing further
Art.
Result of the present invention shows: acrylamide is good in 1～100ng/mL concentration range internal linear, coefficient R2=
0.9999；LOD and LQD is respectively 1.0ng/g, 10.0ng/g；When standard substance pitch-based sphere is 2～80ng/mL, the response rate is
71.58～77.11%, matrix effect is 84.73～95.52%, and relative standard deviation (RSD) is respectively less than 6.0%, and the method has
There is feature accurate, reliable, be suitable to the actually detected of acrylamide in Folium Camelliae sinensis.
Claims (9)
1. a green tea determination of acrylamide, it is characterised in that described assay method is:
(1) sample pre-treatments:
Weighing the green tea sample after pulverizing and be sequentially added into formic acid, isotope labelling acrylamide standard solution, mixing, at 30-90
DEG C water-bath the 10-60min that vibrates；Then it is sequentially added into acetonitrile, magnesium sulfate, sodium chloride, seals vibration, centrifugal；Take supernatant, water
The lower nitrogen of bath dries up, and filters, obtains pretreatment sample；
(2) purify: use solid-phase extraction column that pretreatment sample is carried out purified treatment, obtain testing sample；
(3) use high performance liquid chromatography tandem mass spectrum method that testing sample is detected, calculate acrylamide by internal standard method and contain
Amount.
A kind of green tea determination of acrylamide the most according to claim 1, it is characterised in that: in step (1), described
Isotope labelling acrylamide standard solution is13C3-acrylamide is dissolved in concentration of volume percent 0.1% formic acid and prepares,13C3The concentration of-acrylamide is 30-70ng/mL.
A kind of green tea determination of acrylamide the most according to claim 1 and 2, it is characterised in that: step (1) green tea powder
End, formic acid, the mass volume ratio of isotope labelling acrylamide standard solution are 1g: 7-11mL: 0.8-1.2mL.
A kind of green tea determination of acrylamide the most according to claim 1, it is characterised in that: step (1) green tea powder,
Acetonitrile, magnesium sulfate, the mass volume ratio of sodium chloride are 1g: 9-11mL: 3-5g: 0.5-1.5g.
A kind of green tea determination of acrylamide the most according to claim 1, it is characterised in that: in step (1), pass through
5000-12000rpm r/min is centrifuged 4-10min, takes supernatant, and under 30-90 DEG C of water-bath, nitrogen dries up, through 0.45 μm micropore
Membrane filtration.
A kind of green tea determination of acrylamide the most according to claim 1, it is characterised in that: clean described in step (2)
Change method is: after solid-phase extraction column is carried out pretreatment, and the pretreatment sample that step (1) obtains is carried out loading, and collection passes through
Liquid, crosses film, obtains testing sample.
A kind of green tea determination of acrylamide the most according to claim 1, it is characterised in that: chromatographic determination condition is:
Flowing includes water mutually, mixed liquor and the volumetric concentration of acetonitrile are the formic acid of 0.1%；Flow velocity is 200 μ L/min；Sampling volume 10 μ
L；Column temperature 34-36 DEG C, Qi Zhongshui, acetonitrile mixed liquor in the volume ratio of water and acetonitrile be 99: 1.
A kind of green tea determination of acrylamide the most according to claim 1, it is characterised in that: Mass Spectrometry Conditions: ionizing
Mode is ESI ion source；Scan mode is for just to ionize；Detection mode is polyion reaction monitoring, and collision energy is 8eV, collision
Induction solves ionization voltage: 50V.
Ion source condition: be dried temperature: 325C；Dry gas stream speed: 5L/min；Atomization gas pressure: 45psi；Sheath temperature:
350℃；Sheath gas velocity: 11L/min；Capillary voltage: 3000V, wherein:
9. a kind of green tea determination of acrylamide answering on tea district tea sample is analyzed
With.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113155989A (en) * | 2021-01-28 | 2021-07-23 | 北京理工大学珠海学院 | Rapid detection method for acrylamide content in tea |
| CN114609279A (en) * | 2022-03-10 | 2022-06-10 | 浙江省食品药品检验研究院 | Method for detecting acrylamide in traditional Chinese medicine decoction pieces based on isotope internal standard-QuEChERS-UPLC-MS method |
-
2016
- 2016-05-13 CN CN201610319641.2A patent/CN106124642A/en active Pending
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| Title |
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| JIE LIU ET AL.: "Quantitative analysis of acrylamide in tea by liquid chromatography coupled with electrospray ionization tandem mass spectrometry", 《FOOD CHEMISTRY》 * |
| SANGHEE LEE ET AL.: "In-house–validated liquid chromatography–tandem mass spectrometry (LC-MS/MS) method for survey of acrylamide in various processed foods from Korean market", 《FOOD SCIENCE & NUTRITION》 * |
| 张辉珍等: "食品中丙烯酰胺测定的前处理条件和色谱条件优化", 《食品科学》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113155989A (en) * | 2021-01-28 | 2021-07-23 | 北京理工大学珠海学院 | Rapid detection method for acrylamide content in tea |
| CN114609279A (en) * | 2022-03-10 | 2022-06-10 | 浙江省食品药品检验研究院 | Method for detecting acrylamide in traditional Chinese medicine decoction pieces based on isotope internal standard-QuEChERS-UPLC-MS method |
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Application publication date: 20161116 |
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| RJ01 | Rejection of invention patent application after publication |