CN109324130A - The measuring method of aflatoxin in a kind of tobacco and tobacco product - Google Patents
The measuring method of aflatoxin in a kind of tobacco and tobacco product Download PDFInfo
- Publication number
- CN109324130A CN109324130A CN201811230019.XA CN201811230019A CN109324130A CN 109324130 A CN109324130 A CN 109324130A CN 201811230019 A CN201811230019 A CN 201811230019A CN 109324130 A CN109324130 A CN 109324130A
- Authority
- CN
- China
- Prior art keywords
- aflatoxin
- tobacco
- sample
- measuring method
- tobacco product
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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 invention belongs to tobacco component detection technique fields, and in particular to the measuring method of aflatoxin in a kind of tobacco and tobacco product.Measuring method of the invention is the following steps are included: step 1: preparing the series standard working solution of containing the internal standard and 4 kinds of Aflatoxin B1,B2,G1 and G2s, interior 4 kinds of aflatoxin for being designated as isotope labelling；Step 2: sample to be tested is mixed with internal standard, solvent and sodium chloride, is then extracted, is separated by solid-liquid separation, obtains sample extracting solution；Step 3: sample extracting solution is extracted with the dedicated solid-phase extraction column of aflatoxin, then desorbs and collects stripping liquid as sample prepare liquid；Step 4: series standard working solution and sample prepare liquid are analyzed respectively with liquid chromatography-tandem mass spectrometry.Method purification efficiency of the invention is high, quantitative accurate, applied widely.
Description
Technical field
The invention belongs to tobacco component detection technique fields, and in particular to aflatoxin in a kind of tobacco and tobacco product
Measuring method.
Background technique
Aflatoxin is the derivative of dihydrofuran cumarin, predominantly the secondary metabolism of aspergillus flavus aspergillus parasiticus generation
Product often has in grain, food and the feed under hygrothermal environment.Aflatoxin is a kind of extremely strong violent in toxicity of toxicity
Matter, being delimited by World Health Organization's Agency for Research on Cancer is 1 class carcinogenic substance.Tobacco and correlated product are in storage, transport and processing
It is possible to that mildew can be generated in the process, the safety of tobacco is impacted.The existing laboratory of foreign countries proves higher in water content
Smokeless tobacco in detect aflatoxin, therefore, aflatoxin content pair in Accurate Determining tobacco and tobacco product
Tobacco business is particularly important.
Due to tobacco and the complexity (contain have more than 8000 kinds of compounds altogether) of tobacco product matrix, along with aspergillus flavus poison
Content of the element in above-mentioned sample is possible to lower, it is therefore desirable to a kind of to quantify measuring method accurate, that purification capacity is strong.
In the measuring method of existing aflatoxin content, high performance liquid chromatography-tandem mass has favorable reproducibility, quantitative limit
The advantages that low, high-efficient.It is disclosed in the Chinese patent that Authorization Notice No. is CN104678039B a kind of based on liquid chromatogram-string
The method that connection mass spectrum measures four kinds of aflatoxin contents in tobacco and tobacco product simultaneously, the method achieve yellow bent to four kinds
It is measured while mould toxin.But the content of aflatoxin is extremely low in tobacco and tobacco product, the detection of above method limit compared with
Height, and testing result is affected by operating condition and instrument, therefore the above method cannot be in tobacco and tobacco product
Aflatoxin carries out quantitative well.
Summary of the invention
The purpose of the present invention is to provide a kind of measuring method of aflatoxin in tobacco and tobacco product, this method tools
There are lower detection limit and higher purification efficiency, it is quantitative accurate.
To achieve the above object, the technical scheme is that
The measuring method of aflatoxin in a kind of tobacco and tobacco product, comprising the following steps:
Step 1: preparing the series standard working solution of containing the internal standard and 4 kinds of Aflatoxin B1,B2,G1 and G2s, described interior
It is designated as 4 kinds of Aflatoxin B1,B2,G1 and G2s of isotope labelling；
Step 2: sample to be tested is mixed with internal standard, solvent and sodium chloride, is then extracted, is separated by solid-liquid separation, obtains sample extraction
Liquid；
Step 3: sample extracting solution is extracted with the dedicated solid-phase extraction column of aflatoxin, then desorbs and collects
Stripping liquid is as sample prepare liquid；
Step 4: series standard working solution and sample prepare liquid are analyzed respectively with liquid chromatography-tandem mass spectrometry.
The measuring method of aflatoxin carries out sample extracting solution by extraction in tobacco and tobacco product of the invention
Purification, then scavenging solution is analyzed with liquid chromatography-tandem mass spectrometry instrument, using yellow in internal mark method determination tobacco and tobacco product
The content of aspertoxin.Method of the invention overcomes in existing determination techniques to sample purification without selectivity, purification efficiency
The deficiencies of not high.Every kind of aflatoxin has corresponding Isotopic Internal Standard to be quantified in measuring method of the invention, has
Specific aim.The detection limit of four kinds of aflatoxin is in 0.2 μ g/kg hereinafter, detection limit is low, quantitatively in measuring method of the invention
Accurately.Therefore, method of the invention have many advantages, such as purification efficiency height, high sensitivity, quick and precisely, it is applied widely, can pole
The earth improves testing efficiency, lowering apparatus maintenance cost.
Solvent described in step 2 be methanol aqueous solution or acetonitrile solution, using organic solvent using it is similar mix principle from
Target analytes are leached in tobacco and tobacco product.
To guarantee that the aflatoxin in tobacco and tobacco product is fully extracted, being extracted as being vortexed described in step 2 is mentioned
It takes.
Above-mentioned tobacco product is one of cigarette filler, smoke-free tobacco product, cigar.Method of the invention is suitable
For a variety of tobacco products, use scope is wide.
Chromatographic condition in analytic process described in step 4 are as follows: chromatographic column is HiSep C18-T or equivalent column, chromatogram column temperature
It is 30~40 DEG C, sample volume is 5~20 μ L, and mobile phase A is aqueous formic acid, B is formic acid acetonitrile mixed solution, and flow velocity is
0.2mL/min；Mass Spectrometry Conditions are as follows: electron spray voltage 5000V, atomization gas pressure 50psi, assisted atomization atmospheric pressure 50psi, gas curtain
Atmospheric pressure 35psi, 450 DEG C of ion source temperature, import voltage 8V, exit potential 10V remove cluster voltage 40V, residence time 40ms；
Multiple-reaction monitoring pattern.Method of the invention set instrument parameter in the analysis process, is conducive to improve detection sensitivity.
Separating degree, sensitivity and the disengaging time of 4 kinds of aflatoxin are comprehensively considered, more fast and accurately to be divided
Analysis is as a result, when liquid chromatography-tandem mass spectrometry is analyzed, using isocratic elution, the volume accounting of formic acid in mobile phase A aqueous formic acid
It is 0.05~0.2%, the volume accounting of formic acid is 0.05~0.2% in Mobile phase B formic acid acetonitrile mixture；B body in mobile phase
Product accounting is 30~50%.
For the separation and monitoring convenient for 4 kinds of aflatoxin, sensitivity, liquid chromatography-tandem mass spectrometry point are further increased
When analysis, the quota ion pair of aflatoxin B1 is 313.2/285.2, impact energy 38eV, qualitative ion pair 313.2/
269.2, impact energy 47eV；The quota ion pair of aflatoxin B 2 is 315.2/287.2, impact energy 38eV, it is qualitative from
Son is to for 315.2/271.2, impact energy 51eV；The quota ion pair of aflatoxin G 1 is 329.2/311.1, and impact energy is
38eV, qualitative ion pair 329.2/243.4, impact energy 38eV；The quota ion pair of aflatoxin G 2 is 331.2/
313.2, impact energy 38eV, qualitative ion pair 331.2/245.0, impact energy 47eV.
Detailed description of the invention
Fig. 1 is the multiple-reaction monitoring parameter optimization result of target analytes AFB1 of the invention；
Fig. 2 is the multiple-reaction monitoring parameter optimization result of target analytes AFB2 of the invention；
Fig. 3 is the multiple-reaction monitoring parameter optimization result of target analytes AFG1 of the invention；
Fig. 4 is the multiple-reaction monitoring parameter optimization result of target analytes AFG2 of the invention；
The chromatogram of Fig. 5 is the volume fraction of B phase in mobile phase when being 30% 4 kinds of aflatoxin；
The chromatogram of Fig. 6 is the volume fraction of B phase in mobile phase when being 35% 4 kinds of aflatoxin；
The chromatogram of Fig. 7 is the volume fraction of B phase in mobile phase when being 40% 4 kinds of aflatoxin；
The chromatogram of Fig. 8 is the volume fraction of B phase in mobile phase when being 45% 4 kinds of aflatoxin；
The chromatogram of Fig. 9 is the volume fraction of B phase in mobile phase when being 50% 4 kinds of aflatoxin；
The chromatogram for 4 kinds of aflatoxin that Figure 10 is type of elution when being gradient elution；
Figure 11 is that tobacco sample adds the typical chromatogram obtained after titer in test example 1 of the invention；
Figure 12 is that smokeless tobacco sample adds the typical chromatogram obtained after titer in test example 2 of the invention；
Figure 13 is that cigar sample adds the typical chromatogram obtained after titer in test example 3 of the invention.
Specific embodiment
It is every when being extracted in the measuring method of aflatoxin to sample to be tested in tobacco and tobacco product of the invention
The dosage that 20~30g sample corresponds to solvent is 120~130mL, and the dosage of sodium chloride is 3~7g；The solvent is preferably first
In alcohol solution, the volume ratio of first alcohol and water is (60~80): (20~40).
Extract when institute in tobacco and tobacco product of the invention in the measuring method of aflatoxin to sample to be tested
It could alternatively be potassium chloride with sodium chloride.
When being extracted in the measuring method of aflatoxin to sample extracting solution in tobacco and tobacco product of the invention
Extraction column used is the dedicated solid-phase extraction column of aflatoxin, is Romer AflaStar Aspergillus flavus toxin immuno-affinity column
Aflatoxin dedicated columns (the 100mg/ of (3mL, product number COIAC1001) or Weitaike Technology (Wuhan) Co., Ltd.
3mL, product number 27-01003).
In order to obtain higher sensitivity, the present invention instrument parameter and condition that influence testing result investigate and
Optimization specifically includes the multiple-reaction monitoring parameter (quota ion pair and collision energy etc.) for influencing detection sensitivity and influences separation
The mobile phase condition of effect.
The optimum results of multiple-reaction monitoring parameter are as shown in Figure 1 to 4, and detailed process is after determining parent ion 10
Daughter ion scanning (wherein the scanning range of daughter ion is 50~mother ion mass-to-charge ratio) is carried out within the scope of~90eV, and then determines two
A highest ion pair of respective strengths and corresponding impact energy, respectively as quota ion pair and qualitative ion pair.From Fig. 1~figure
4 can be seen that under the conditions of the parent ion optimized, the daughter ion that 4 kinds of aflatoxin obtain under different impact energies
Type and intensity are also different, and the final selected multiple-reaction monitoring parameter of the present invention is as shown in table 1.
1 target analytes of table and interior target multiple-reaction monitoring parameter list
For mobile phase by A phase and B phase composition, A phase is preferably the formic acid solution of 0.1vol%, and B phase is preferably formic acid and acetonitrile
The mixed solution of composition, wherein the volume accounting of formic acid is 0.1%.
The mobile phase for choosing the B phase of the score containing different volumes carries out isocratic elution and is tested, specific test result such as Fig. 5
Shown in~Fig. 9.With the increase of formic acid acetonitrile (B phase) volume fraction in mobile phase, the reservation of 4 kinds of target analytes is increasingly
It is weak, while the separating effect of C18 chromatographic column is also gradually deteriorated, this is because caused by the hydrophobic property of aflatoxin.
It is tested using gradient elution, condition of gradient elution program is respectively t=0min, 30%B, t=10.0min,
40%B, t=12.0min, 40%B, t=12.1min, 30%B, t=20.0min, 30%B, specific test result such as Figure 10 institute
Show.It can be seen that the separating effect of target analytes has a degree of improvement under condition of gradient elution, but object
Half-peak breadth it is larger, be unfavorable for the raising of sensitivity；Simultaneously compared with isocratic elution, the chromatographic isolation time of gradient elution has
Increase.
Therefore comprehensively consider separating degree, sensitivity and disengaging time, mobile phase carries out isocratic elution using 60%A-40%B
Effect it is best.
The embodiment 1 of the measuring method of aflatoxin
The present embodiment is the measuring method of aflatoxin in tobacco and tobacco product, using the aflatoxin of optimization
Analysis condition, specifically includes the following steps:
Step 1: using acetonitrile as solvent, the series standard work of containing the internal standard and 4 kinds of Aflatoxin B1,B2,G1 and G2s is prepared
Make solution, wherein in be designated as C13 isotope labelling 4 kinds of aflatoxin (be denoted as respectively [13C17]-AFB1、[13C17]-AFB2、
[13C17]-AFG1 and [13C17]-AFG1)；The concentration gradient of 4 kinds of aflatoxin is 0.5 μ g/ in series standard working solution
Kg, 1.0 μ g/kg, 2.0 μ g/kg, 5.0 μ g/kg, 10.0 μ g/kg, 20.0 μ g/kg and 50.0 μ g/kg, C13 isotope labellings 4
Concentration of the kind aflatoxin in series standard working solution is 5.0 μ g/kg；
Step 2: to 25g drying, the second for crushing, sequentially adding 0.25mL containing the internal standard in the tobacco of sieving and tobacco product
Nitrile solution (wherein the concentration of 4 kinds of aflatoxin of C13 isotope labelling is 500ng/mL), 125mL methanol-water (volume
Than the mixed extract and 5.0g sodium chloride for 7:3), extraction of ocean eddies 2.0min, then it is centrifuged with revolving speed for the speed of 4000rpm
5min is taken supernatant liquor to be diluted with the water of its 2 times of volumes, is filtered with glass microfibre filter paper, collects filtrate as sample extraction
Liquid；
Step 3: 15.0mL sample extracting solution is slowly flowed across into the dedicated solid-phase extraction column (Romer of aflatoxin
AflaStar Aspergillus flavus toxin immuno-affinity column (3mL, product number COIAC1001)), after waiting sample extracting solutions to flow completely out,
Filler 2 times for having adsorbed object and interfering substance are cleaned with 10.0mL pure water, and are sucked out or squeeze out cleaning solution therein；It uses again
The desorption of 1.0mL methanol collects stripping liquid as sample prepare liquid；
Step 4: respectively analyzing series standard working solution and sample prepare liquid with liquid chromatography-tandem mass spectrometry,
Chromatographic condition in analytic process are as follows: chromatographic column is HiSep C18-T (2.1 × 150mm, 5 μm), and chromatogram column temperature is 40 DEG C, into
Sample amount is 10 μ L, and by A phase and B phase, 60:40 is formed mobile phase by volume, and the formic acid solution that A phase is 0.1vol%, B phase is first
The mixed solvent of acid and acetonitrile composition, the volume accounting of formic acid are 0.1%, flow velocity 0.2mL/min；Mass Spectrometry Conditions are as follows: EFI
Mist voltage 5000V, atomization gas pressure 50psi, assisted atomization atmospheric pressure 50psi, gas curtain atmospheric pressure 35psi, ion source temperature 450
DEG C, import voltage 8V, exit potential 10V remove cluster voltage 40V, residence time 40ms；Multiple-reaction monitoring pattern；
Step 5: it is quantified by the ratio between the peak area of 4 kinds of aflatoxin and internal standard peak area, specific operation process
Are as follows: with the ratio between the peak area of 4 kinds of aflatoxin in series standard working solution and corresponding internal standard peak area for ordinate, series
The concentration of 4 kinds of aflatoxin is abscissa in standard working solution, draws working curve respectively；According to 4 in sample prepare liquid
Kind of the ratio between aflatoxin peak area and corresponding internal standard peak area obtain in sample 4 kinds of aflatoxin according to working curve
Content, its calculation formula isWherein x is the ratio between object and the peak area of internal standard compound, and m is in sample
The content (unit is μ g/kg) of object, a and b are slope and intercept in working curve, are found out by working curve, V is to mention
The volume (unit mL) of liquid is taken, n is sample quality (unit kg).
The detection of the measuring method of aflatoxin limits and is quantitatively limited to 4 kinds in tobacco and tobacco product in the present embodiment
Corresponding concentration when aflatoxin signal-to-noise ratio (S/N) is 3 and 10, the range of linearity of the method for the present embodiment, working curve,
Detection limit and quantitative limit are as shown in table 2.
2 range of linearity of table, working curve, detection limit and quantitative limit
Test example 1
In order to investigate embodiment 1 method repeatability and accuracy, into sample to be tested add various concentration 4 kinds of Huangs
Aspertoxin mixed solution (concentration is respectively 0.5 μ g/kg, 5.0 μ g/kg and 20.0 μ g/kg) carries out Solid Phase Extraction afterwards, then into
Row analysis.Concrete analysis process are as follows: replicate analysis 4 times in 1d are calculated actually detected value by working curve, and calculate not
With the rate of recovery under concentration and in a few days relative standard deviation；It is measured, is calculated under various concentration with sample prepared by continuous 3d
The rate of recovery and relative standard deviation in the daytime.The results are shown in Table 3.
The rate of recovery and precision under 3 various concentration of table
As shown in Table 3, recovery of standard addition of the target analytes under various concentration be 90.1%~113.6%, in a few days and
Day to day precision is not more than 9.6% and 10.8% respectively, it was demonstrated that the survey of aflatoxin in tobacco and tobacco product of the invention
Determining method has preferable repeatability and stability.
Test example 2
Method referring to the embodiment 1 of the measuring method of aflatoxin in tobacco and tobacco product is (roasting to tobacco sample
Cigarette tobacco leaf, grade C3F) it is analyzed, the results showed that the 4 kinds of aflatoxin studied in tobacco sample without the present invention.For
The accuracy of further verifying this method, adds the mixed solutions of 4 kinds of aflatoxin as titer in tobacco sample,
Its concentration is 5.0 μ g/kg, later referring to the measurement of the embodiment 1 of the measuring method of aflatoxin in tobacco and tobacco product
Method is tested and analyzed.Actual sample adds the typical chromatogram obtained after titer as shown in figure 11, it can be seen that target point
Analysis object separates well with chaff interferent, and interfering substance does not influence quantifying for object；Its recovery of standard addition and precision such as 4 institute of table
Show.
The recovery of standard addition and precision of target analytes in 4 tobacco sample of table
| Analyte | The rate of recovery ± RSD% (n=4) |
| AFB1 | 96.3±1.6 |
| AFB2 | 106.6±2.2 |
| AFG1 | 91.1±4.4 |
| AFG2 | 105.0±2.5 |
As shown in table 4, the relative recovery of target analytes shows the present invention between 91.1-106.6% in sample
Method accuracy it is good, can satisfy the analysis requirement of aflatoxin in daily tobacco sample.
Test example 3
The measuring method of the embodiment 1 of the measuring method of aflatoxin is to smokeless cigarette in reference tobacco and tobacco product
Straw-made articles is analyzed, and smoke-free tobacco product used is CRP1.1.The result shows that without this method research in institute's sample
4 kinds of aflatoxin.In order to further verify the accuracy of this method, the mixing for adding 4 kinds of aflatoxin in the sample is molten
For liquid as titer, concentration is 5.0 μ g/kg, later referring to the measuring method of aflatoxin in tobacco and tobacco product
The measuring method of embodiment 1 is tested and analyzed.Actual sample adds the typical chromatogram obtained after titer as shown in figure 12, can
It is separated well with seeing target analytes with chaff interferent, interfering substance does not influence quantifying for object；Its recovery of standard addition and essence
Density is as shown in table 5.
The recovery of standard addition and precision of target analytes in 5 smokeless tobacco sample of table
| Analyte | The rate of recovery ± RSD% (n=4) |
| AFB1 | 89.0±3.8 |
| AFB2 | 98.0±3.1 |
| AFG1 | 90.5±3.4 |
| AFG2 | 104.3±3.6 |
As shown in table 5, the relative recovery of target analytes shows the present invention between 89.0-104.3% in sample
Method accuracy it is good, can satisfy the analysis requirement of aflatoxin in daily smokeless tobacco sample.
Test example 4
The measuring method of the embodiment 1 of the measuring method of aflatoxin is to cigar sample in reference tobacco and tobacco product
Product are analyzed, and sample used is villiger PREMIUN NO.1 (Willie 1).The result shows that without this in institute's sample
4 kinds of aflatoxin of technique study.In order to further verify the accuracy of this method, 4 kinds of aspergillus flavus poison are added in the sample
For the mixed solution of element as titer, addition concentration is 5.0 μ g/kg, later referring to aspergillus flavus poison in tobacco and tobacco product
The measuring method of the embodiment 1 of the measuring method of element is tested and analyzed.Actual sample adds the typical chromatography obtained after titer
Figure is as shown in figure 13, it can be seen that under optimal conditions, target analytes separate well with chaff interferent, and interfering substance does not influence
Object quantifies；Its recovery of standard addition and precision are as shown in table 6.
The recovery of standard addition and precision of target analytes in 6 cigar sample of table
| Analyte | The rate of recovery ± RSD% (n=4) |
| AFB1 | 96.8±4.3 |
| AFB2 | 96.6±5.3 |
| AFG1 | 102.0±2.1 |
| AFG2 | 106.6±2.0 |
As shown in table 6, the relative recovery of target analytes shows the present invention between 96.6-106.6% in sample
Method accuracy it is good, can satisfy the analysis requirement of aflatoxin in daily cigar sample.
Claims (7)
1. the measuring method of aflatoxin in a kind of tobacco and tobacco product, which comprises the following steps:
Step 1: preparing the series standard working solution of containing the internal standard and 4 kinds of Aflatoxin B1,B2,G1 and G2s, it is described in be designated as
4 kinds of Aflatoxin B1,B2,G1 and G2s of isotope labelling；
Step 2: sample to be tested is mixed with internal standard, solvent and sodium chloride, is then extracted, is separated by solid-liquid separation, obtains sample extracting solution；
Step 3: sample extracting solution is extracted with the dedicated solid-phase extraction column of aflatoxin, then desorbs and collects desorption
Liquid is as sample prepare liquid；
Step 4: series standard working solution and sample prepare liquid are analyzed respectively with liquid chromatography-tandem mass spectrometry.
2. according to claim 1 in tobacco and tobacco product aflatoxin measuring method, which is characterized in that step 2
The solvent is methanol aqueous solution or acetonitrile solution.
3. the measuring method of aflatoxin in tobacco according to claim 1 or claim 2 and tobacco product, which is characterized in that step
Extraction of ocean eddies is extracted as described in rapid two.
4. according to claim 1 in tobacco and tobacco product aflatoxin measuring method, which is characterized in that the cigarette
Straw-made articles is one of cigarette filler, smoke-free tobacco product, cigar.
5. according to claim 1 in tobacco and tobacco product aflatoxin measuring method, which is characterized in that step 4
Chromatographic condition in the analytic process are as follows: chromatographic column is HiSep C18-T or equivalent column, and chromatogram column temperature is 30~40 DEG C, into
Sample amount is 5~20 μ L, and mobile phase A is aqueous formic acid, Mobile phase B is formic acid acetonitrile mixed solution, flow velocity 0.2mL/min；
Mass Spectrometry Conditions are as follows: electron spray voltage 5000V, atomization gas pressure 50psi, assisted atomization atmospheric pressure 50psi, gas curtain atmospheric pressure
35psi, 450 DEG C of ion source temperature, import voltage 8V, exit potential 10V remove cluster voltage 40V, residence time 40ms；More reactions
Monitoring pattern.
6. according to claim 5 in tobacco and tobacco product aflatoxin measuring method, which is characterized in that liquid phase color
When spectrum-Tandem Mass Spectrometry Analysis, using isocratic elution, in mobile phase A aqueous formic acid the volume accounting of formic acid be 0.05~
0.2%, the volume accounting of formic acid is 0.05~0.2% in Mobile phase B formic acid acetonitrile mixture；Mobile phase B volume accounting is 30
~50%.
7. according to the measuring method of aflatoxin in the tobacco of claim 5 or 6 and tobacco product, which is characterized in that liquid
When phase chromatography-Tandem Mass Spectrometry Analysis, the quota ion pair of aflatoxin B1 is 313.2/285.2, impact energy 38eV, qualitative
Ion pair is 313.2/269.2, impact energy 47eV；The quota ion pair of aflatoxin B 2 is 315.2/287.2, impact energy
For 38eV, qualitative ion pair 315.2/271.2, impact energy 51eV；The quota ion pair of aflatoxin G 1 is 329.2/
311.1, impact energy 38eV, qualitative ion pair 329.2/243.4, impact energy 38eV；Aflatoxin G 2 it is quantitative from
Son is to for 331.2/313.2, impact energy 38eV, qualitative ion pair 331.2/245.0, impact energy 47eV.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811230019.XA CN109324130A (en) | 2018-10-22 | 2018-10-22 | The measuring method of aflatoxin in a kind of tobacco and tobacco product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811230019.XA CN109324130A (en) | 2018-10-22 | 2018-10-22 | The measuring method of aflatoxin in a kind of tobacco and tobacco product |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109324130A true CN109324130A (en) | 2019-02-12 |
Family
ID=65262644
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811230019.XA Pending CN109324130A (en) | 2018-10-22 | 2018-10-22 | The measuring method of aflatoxin in a kind of tobacco and tobacco product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109324130A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110609107A (en) * | 2019-09-16 | 2019-12-24 | 宁波立华制药有限公司 | Method for detecting aflatoxins G2, G1, B2 and B1 in radix paeoniae alba decoction pieces by using ultra-high performance liquid chromatography-mass spectrometry |
| CN113219092A (en) * | 2021-04-29 | 2021-08-06 | 中国烟草总公司湖北省公司 | Method for simultaneously measuring multiple aflatoxins in tobacco leaves by dispersion liquid-liquid microextraction-high performance liquid chromatography-tandem mass spectrometry |
| CN113252818A (en) * | 2021-07-07 | 2021-08-13 | 裕菁科技(上海)有限公司 | Method for quantifying and evaluating compounds of same series by adopting reference sample |
| CN114460210A (en) * | 2022-01-29 | 2022-05-10 | 国家粮食和物资储备局科学研究院 | Kit and method for detecting various mycotoxins with high precision |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104678039A (en) * | 2015-01-30 | 2015-06-03 | 湖南中烟工业有限责任公司 | Method for simultaneously measuring contents of four aflatoxins in tobacco and tobacco products by liquid chromatography-tandem mass spectrometry combination |
-
2018
- 2018-10-22 CN CN201811230019.XA patent/CN109324130A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104678039A (en) * | 2015-01-30 | 2015-06-03 | 湖南中烟工业有限责任公司 | Method for simultaneously measuring contents of four aflatoxins in tobacco and tobacco products by liquid chromatography-tandem mass spectrometry combination |
Non-Patent Citations (2)
| Title |
|---|
| SHAHZAD ZAFAR IQBAL ET AL.: "Aflatoxins contamination in peanut and peanut products commercially available in retail markets of Punjab, Pakistan", 《FOOD CONTROL》 * |
| 彭康年 等: "液相色谱-串联质谱法测定动物肝脏中黄曲霉毒素", 《分析科学学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110609107A (en) * | 2019-09-16 | 2019-12-24 | 宁波立华制药有限公司 | Method for detecting aflatoxins G2, G1, B2 and B1 in radix paeoniae alba decoction pieces by using ultra-high performance liquid chromatography-mass spectrometry |
| CN113219092A (en) * | 2021-04-29 | 2021-08-06 | 中国烟草总公司湖北省公司 | Method for simultaneously measuring multiple aflatoxins in tobacco leaves by dispersion liquid-liquid microextraction-high performance liquid chromatography-tandem mass spectrometry |
| CN113252818A (en) * | 2021-07-07 | 2021-08-13 | 裕菁科技(上海)有限公司 | Method for quantifying and evaluating compounds of same series by adopting reference sample |
| CN114460210A (en) * | 2022-01-29 | 2022-05-10 | 国家粮食和物资储备局科学研究院 | Kit and method for detecting various mycotoxins with high precision |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109324130A (en) | The measuring method of aflatoxin in a kind of tobacco and tobacco product | |
| CN107884493A (en) | The method of short chain chlorinated paraffin in comprehensive two dimensional gas chromatography flying time mass spectrum analysis environmental sample | |
| CN106124674A (en) | The pre-treating method of a kind of quick mensuration Pesticide Residues in Tea and quantitative analysis method | |
| CN1332199C (en) | GC/MS inner scaling detection method for simultaneous investigating residual multiple organophosphorus in food | |
| CN106093248A (en) | Levoglucosan, mannan and the method for galactan in high performance liquid chromatography QQ-TOF mass spectrometry combination Simultaneous Determination aerosol | |
| Rodin et al. | Determination of the products of the oxidative transformation of unsymmetrical dimethylhydrazine in soils by liquid chromatography/mass spectrometry | |
| CN103308641A (en) | High performance liquid chromatography-tandem mass spectrometry measuring method of three amide herbicides in tobacco and tobacco products | |
| CN111089931A (en) | Detection method of parecoxib sodium gene genotoxicity impurity | |
| CN111830141A (en) | Method for screening pesticide residues in medicine-food homology food by using pesticide residue mass spectrum database | |
| CN111679008A (en) | GC-MS-MS method for simultaneously detecting volatile and semi-volatile acids, alcohols and phenols in tobacco leaves and cut tobacco | |
| CN109212054B (en) | Method for determining tomatidine by high performance liquid chromatography-mass spectrometry | |
| CN107037151B (en) | A kind of measuring method of transfer volume of epoxy chloropropane in food contact material | |
| Zhao-Yong et al. | Rapid screening and identification of paralytic shellfish poisoning toxins in red tide algae using hydrophilic interaction liquid chromatography-high resolution mass spectrometry with an accurate-mass database | |
| CN107064364A (en) | The assay method of Performance Liquid Chromatography Analysis for Nicotine in Tobacco optical isomer | |
| CN109324129A (en) | A kind of method of aflatoxin in measurement electronic cigarette liquid | |
| CN103558312B (en) | Method for measuring benzo[a]pyrene content of mainstream smoke of cigarettes | |
| CN108562664A (en) | A kind of method of the triple level four bars of liquid chromatogram-- linear ion hydrazine mass spectrum to more pesticide residue determinations in food | |
| CN105938102B (en) | Method for rapidly determining pesticide residues in fruits and vegetables by chemical color development method | |
| Vázquez et al. | Application of coupled-column liquid chromatography combined with post-column photochemically induced fluorimetry derivatization and fluorescence detection to the determination of pyrethroid insecticides in vegetable samples | |
| CN109324131A (en) | The measuring method of aflatoxin in a kind of Cigarette paper | |
| CN1261749C (en) | Method for rapidly and quantitatively determining the triterpenoid content in ganoderma lucidum | |
| CN114236026A (en) | Non-targeting rapid screening method for pesticide residues in fruits and vegetables | |
| CN108828101B (en) | Method for determining diuron residues in sugarcane based on 3, 4-dichloroaniline | |
| CN103091438B (en) | Method for measuring benzo [a] pyrene content in cigarette filter | |
| CN115128177A (en) | Method for analyzing and determining genotoxic impurities in ganciclovir condensation compound by using HPLC method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190212 |
|
| RJ01 | Rejection of invention patent application after publication |