CN105974018A - Method for detecting toxoflavin in foodstuff based on multifunctional purifying column-high performance liquid chromatography - Google Patents
Method for detecting toxoflavin in foodstuff based on multifunctional purifying column-high performance liquid chromatography Download PDFInfo
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Abstract
The invention provides a method for detecting a toxoflavin residue in foodstuff based on multifunctional purifying column purification-high performance liquid chromatography. 80mL of acetonitrile and 20mL of water are used for dissolving a foodstuff sample, ultrasonic extraction is carried out, a multifunctional purifying column is used for purifying, 5.0mL of purifying liquid is used, N2 is used for blowing and drying, 1.0mL of water is used for metering the volume, and liquid for testing is obtained. Detection of the toxoflavin residue in the sample is realized, and the method has the advantages of good purifying effects, accurate quantification, and elimination of influences of solvent effect on chromatographic behaviors of toxoflavin. Gradient elution of a mobile phase is carried out by methanol and water, retention of toxoflavin in a reversed phase chromatography column, effective separation between toxoflavin and other interfering substances is realized during sample analysis, so that the purpose of accurate quantification is realized. In the sample purifying process, interferences of lipids, pigments, proteins and other substances are effectively removed from the sample, the purifying effect is good, and the quantitative analysis has good accuracy, high sensitivity, and good result reappearance; and the method is suitable for detection of the toxoflavin residue in a plurality of foodstuffs.
Description
Technical field
The present invention relates to technical field of food safety, particularly relate to a kind of based on Multifunctional cleanup column-high performance liquid chromatography
The method of method detection alimentary toxicosis flavin.
Background technology
The structural formula of toxoflavin (toxoflavin) (CAS:84-82-2) is:
It is a kind of bacteriotoxin causing alimentary toxicosis produced by Pseudomonas cocovenenans subsp farinofermantans.Common
Contaminated food products is mainly frumentum fermented product, potato based article and Tremella etc..Pseudomonas cocovenenans subsp farinofermantans alimentary toxicosis is many
Occur, in overcast and rainy moist season in autumn in summer (main 5～August), to cause Pseudomonas cocovenenans Fast-propagation because food storage is improper
Growth, eats and can be caused poisoning by its food polluted, show as the diseases such as epigastric discomfort, Nausea and vomiting, dizziness and general weakness
Shape, seriously may occur in which hepatosplenomegaly, subcutaneous hemorrhage, hematuria and shock etc., and mortality rate is up to 40～100%.For many years about coconut palm
The report of the poison pseudomonas poisoning a lot of death of initiation is more, is found in the alimentary toxicosis that nineteen fifty-three fermented flour causes the earliest, after
The most all it is found to have the food poisoning that Pseudomonas cocovenenans causes.Slurry cake " is hung " in Guangnan in 2014, and coconut palm poison is false
Zymomonas mobilis food poisoning just causes many people dead, and the Spring Festival in 2015, Liaoyang occurred Suantangzi poisoning, doubted because of rice yeast-like fungi
Acid and toxoflavin poisoning induced 4 people are dead.
Currently, with respect to the detection method of toxoflavin, there is no corresponding national standard or industry standard.Recent domestic closes
In the research of alimentary toxicosis flavin detection technique, also rarely has report.
Summary of the invention
Present invention aims to the deficiency of existing detection technique, it is provided that a kind of side detecting alimentary toxicosis flavin
Method.The present invention can detect frumentum fermented product and (include fermented maize face, glutinous rice flour, hangs slurry cake, corn starch, vinegar bean jelly
Deng), Tremella and the alimentary toxicosis flavin such as goods, potato based article (such as Rhizoma Solani tuber osi bean noodles, sweet potato starch, sweet potato starch etc.) residual
Stay.
It is an object of the invention to be achieved through the following technical solutions: a kind of based on the liquid phase of Multifunctional cleanup column-efficiently
The method of chromatography detection alimentary toxicosis flavin, comprises the following steps:
(1) sample extraction condition: after weighing 20～25g samples and 100mL extracting solution (80 acetonitrile+20 water) mixing, ultrasonic
Extracting 30min, take extracting solution, 5000r/min is centrifuged 5min, obtains supernatant.
(2) sample purification: take the supernatant 10mL that step 1 obtains, crosses Multifunctional cleanup column and purifies；After purification, take
Scavenging solution 5.0mL N2 dries up, then with 1.0mL pure water constant volume, obtains upper machine liquid after vortex dissolving.
(3) chromatographiccondition: upper machine liquid step 2 obtained quarternary low pressure or binary through being furnished with DAD detector is high
Pressure liquid chromatography system carries out chromatography, chromatographic column: ODS reversed phase chromatographic column (such as ODS C18), 250*4.6mm, 5 μm；Stream
Move and be mutually: methanol and water gradient elution, volume ratio is (0～10min, 7:93；10.1～20min, 98:2；20.1～27min,
7:93)；Sample size: 20 μ L；Flow velocity: 1.0mL/min；Column temperature: 30 DEG C.Detection wavelength: 258nm.
(4) qualitative analysis of samples: the retention time obtained according to step 3 chromatography and characteristic light spectrogram, with standard specimen
Retention time and characteristic light spectrogram are compared, if both coincide, then show containing toxoflavin.
(5) sample amounts analysis: standard specimen is prepared: toxoflavin is dissolved in water, is configured to concentration and is respectively 0.05,0.1,0.2,
0.4,1.0,2.0,5.0,10.0 μ g/mL series standard uses liquid.Using standard specimen response peak area as vertical coordinate, standard specimen concentration it is
Abscissa (μ g/mL), draws calibration trace.The response peak area obtained according to step 3 chromatography, uses external standard method, to sample
In product, toxoflavin content carries out quantitative analysis.
Further, described concentration is respectively 0.05,0.1,0.2,0.4,1.0,2.0,5.0,10.0 μ g/mL series standard
The compound method using liquid is as follows: weigh 0.0100g toxoflavin standard substance in 10mL volumetric flask, after methanol dissolves, is settled to
Scale, is configured to 1.0mg/mL standard mother solution.It is positioned in-18 DEG C of refrigerators, can preserve 3 months.Before using, take out holding chamber
Wen Hou, takes 200 μ L standard mother solutions in 10mL volumetric flask, and water is settled to scale, shakes up, and is configured to the middle chien shih of 20.0 μ g/ml
Use liquid.Take respectively and in the middle of 25 μ L, 50 μ L, 100 μ L, 200 μ L, 500 μ L, 1.0mL, use liquid and 50 μ L, 100 μ L standard mother solutions
In 10mL volumetric flask, water is settled to scale.
Further, described detection food is that frumentum fermented product (includes fermented maize face, glutinous rice flour, hangs slurry cake, Semen Maydis
Starch, vinegar bean jelly etc.), Tremella and goods, potato based article (such as Rhizoma Solani tuber osi bean noodles, sweet potato starch, sweet potato starch etc.) etc..
The invention has the beneficial effects as follows, use a kind of detection efficiency height, clean-up effect and the response rate to disclosure satisfy that detection is wanted
The solid phase extraction techniques asked, by optimizing extraction conditions (Extraction solvent and extraction time) in pretreatment process, selects 80% second
Nitrile water (volume ratio) is as the extraction reagent of toxoflavin, supersound extraction 30min in sample, it is achieved that object toxoflavin abundant
Extract, decrease highly polar impurity component (pigment, fat and other interfering components etc.) and in chromatography, toxoflavin is done
Disturb.It addition, chromatographic condition is improved by the present invention, establish and the most effectively achieve for flowing with first alcohol and water gradient elution
During sample detection, target analytes toxoflavin separates with other interfering components.The present invention is in actually detected, and Solid Free extracts
Pillar activation and elution step, detection efficiency is high, and good purification is highly sensitive, it is easy to popularization and application, and is applicable to multiple food
Toxoflavin retention analysis in product sample.
Accompanying drawing explanation
Fig. 1 is calibration trace (Y=142529.9x+12501.41, the R of standard specimen2=0.9998, R=0.9999)；
Fig. 2 is toxoflavin standard specimen chromatogram (retention time is 10.785min)；
Fig. 3 is toxoflavin spectrogram；
Fig. 4 is the chromatogram that 80% methanol-water dissolves toxoflavin；
Fig. 5 is the chromatogram that 90% methanol dissolves toxoflavin；
Fig. 6 is the chromatogram that 100% methanol dissolves toxoflavin；
Fig. 7 is fermented maize face sample chromatogram figure (negative)；
Fig. 8 is fermented maize face sample spectrum diagram (corresponding retention time is 10.331min)；
Fig. 9 be the methanol-water of volume fraction 70% be chromatogram during Extraction solvent (crossing column purification)；
Figure 10 be the ethanol water of volume fraction 70% be chromatogram during Extraction solvent (crossing column purification)；
Figure 11 be the acetonitrile water of volume fraction 70% be chromatogram during Extraction solvent (crossing column purification)；
Figure 12 be the acetonitrile water of volume fraction 80% be the chromatogram (but column purification) during Extraction solvent；
Figure 13 be the acetonitrile water of volume fraction 80% be chromatogram during Extraction solvent (crossing column purification)；
Figure 14 be pitch-based sphere be the fermented maize complexion spectrogram of 0.1mg/kg；
Figure 15 be pitch-based sphere be the fermented maize complexion spectrogram of 0.5mg/kg；
Figure 16 be pitch-based sphere be the fermented maize complexion spectrogram of 1.5mg/kg；
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1: draw the calibration trace of response peak area-toxoflavin concentration.
(1) weigh 0.0100g toxoflavin standard substance in 10mL volumetric flask, after methanol dissolves, be settled to scale, be configured to
1.0mg/mL standard mother solution.It is positioned in-18 DEG C of refrigerators, can preserve 3 months.Before using, take out after placing room temperature, take 200 μ
L standard mother solution is in 10mL volumetric flask, and water is settled to scale, shakes up, and is configured to the middle of 20.0 μ g/ml and uses liquid.Take respectively
25 μ L, 50 μ L, 100 μ L, 200 μ L, use liquid and 50 μ L in the middle of 500 μ L, 1.0mL, 100 μ L standard mother solutions are in 10mL capacity
In, water is settled to scale.It is configured to concentration and is respectively 0.05,0.1,0.2,0.4,1.0,2.0,5.0,10.0 μ g/ml series mark
Quasi-use liquid.
Meanwhile, constant volume solution is optimized by this part, compares different volumes mark methanol-water (0～100%) right
The impact of toxoflavin chromatographic behavior.Find the methanol aqueous solution (Fig. 4) of volume fraction 80%, 90% methanol aqueous solution (Fig. 5),
100% methanol (Fig. 6) is more significant to the adverse effect of toxoflavin chromatographic behavior in chromatography.Methanol volume in constant volume solution
During mark more than 80%, when chromatography, toxoflavin chromatographic peak forms two bifurcated peaks.From structural analysis, toxoflavin is
Middle polarity compound, solvent effect is strong, use highly polar water as constant volume solvent can eliminate toxoflavin solvent effect thus
Form sharp-pointed symmetrical chromatographic peak.Owing under toxoflavin acid condition, (pH < when 2) is unstable, this study portion is at flowing phase bar
Part and constant volume solution are all provided without organic acid.
(2) using standard specimen response peak area as vertical coordinate, standard specimen concentration is abscissa (μ g/mL), draws calibration trace.As
Shown in Fig. 1.Retention time as in figure 2 it is shown, characteristic light spectrogram as shown in Figure 3.
Embodiment 2: the present embodiment detects the toxoflavin in fermented maize face by the following method:
(1) sample extraction condition: after weighing 20～25g samples and 100mL extracting solution (80 acetonitrile+20 water) mixing, ultrasonic
Extracting 30min, take extracting solution, 5000r/min is centrifuged 5min, obtains supernatant.
(2) sample purification: take the supernatant 10mL that step 1 obtains, crosses Multifunctional cleanup column and purifies；After purification, take
Scavenging solution 5.0mL N2Dry up, then with 1.0mL pure water constant volume, after vortex dissolving, obtain upper machine liquid.
(3) chromatographiccondition: upper machine liquid step 2 obtained quarternary low pressure or binary through being furnished with DAD detector is high
Pressure liquid chromatography system carries out chromatography, chromatographic column: ODS reversed phase chromatographic column (such as ODS C18), 250*4.6mm, 5 μm；Stream
Move and be mutually: methanol and water gradient elution ((0～10min, 7:93；10.1～20min, 98:2；20.1～27min, 7:93)；Enter
Sample amount: 20 μ L；Flow velocity: 1.0mL/min；Column temperature: 30 DEG C.Detection wavelength: 258nm.
This semiconvection is moved phase condition and is optimized, and compares when adding a certain proportion of acetic acid in flowing mutually yellow to poison
The impact that plain color spectrum retains.Acetic acid belongs to highly polar organic acid, adds acetic acid and be equivalent to enhance the polarity of flowing phase in flowing mutually,
Thus decrease toxoflavin retention time in reversed phase chromatographic column, it is unfavorable for toxoflavin and interfering compound during sample analysis
Separate.This part uses first alcohol and water gradient elution flowing phase, beneficially middle polarity compound toxoflavin and other interferenceization
Efficiently separating of compound, thus reach the purpose of accurate quantitative analysis.
(4) qualitative analysis of samples: according to step 3 chromatography, the retention time obtained as described in Figure 7, characteristic light spectrogram
As shown in Figure 8, the retention time (Fig. 2) of standard specimen obtained with embodiment 1 and characteristic light spectrogram (Fig. 3) find after comparing,
In the present embodiment, fermentation rice and flour characteristic light spectrogram (Fig. 8) of detection is misfitted with the characteristic light spectrogram (Fig. 3) of standard specimen, shows not contain
There is toxoflavin.
Embodiment 3: the present embodiment is in example 2, simultaneously positive by adding the preparation of toxoflavin standard substance in Semen Maydis flour
Fermented maize face sample is a, and detects by same procedure.Wherein in step 1, this part is tried extracting reagent
Test, have selected the methanol-water (Fig. 9) of equal volume mark 70%, 70% ethanol water (Figure 10) and 70% acetonitrile water (Figure 11), examine
Examine different organic solvents on the impact of extraction efficiency and on multifunctional purifying column purification, the impact of recovering effect.Wherein, difference has
Machine solvent on the impact of extraction efficiency by positive corn fermentation face extracted after, take respectively the direct N2 of 3.0ml extracting solution dry up,
Machine analysis on water dissolution, thus got rid of the response rate impact that column purification brings.It addition, respectively take extracting section liquid respectively by many
Function decontaminating column purifies, and investigates the purification of different solvents, the response rate further.Concrete outcome is shown in Table 1.By accompanying drawing 9,
10,11 and table 1 it can be seen that under equal volume mark, the extraction efficiency of acetonitrile and the purification of Multifunctional cleanup column, recovering effect
It is better than methanol and ethanol.
The toxoflavin content (representing with peak area) that table 1 different solvents records when extracting
| Organic solvent volume mark | 70% methanol-water | 70% ethanol water | 70% acetonitrile water |
| Peak area (but post) | 82047 | 73708 | 97234 |
| Peak area (crosses post) | 42664 | 31957 | 60285 |
| Response rate % | 52.0 | 43.4 | 62.0 |
Embodiment 4: the present embodiment in embodiment 3, have studied different volumes mark acetonitrile water to extraction simultaneously to step 1
The impact of efficiency.Fermented maize face have selected 10%～100% acetonitrile water, by supersound extraction 30min, by centrifugation after, respectively
Take 3.0mL extracting solution through N2Dry up, 1.0ml water constant volume post analysis.Result is as shown in table 2.Find Extraction solvent acetonitrile volume integral
Extraction efficiency the highest (Figure 12) when number is 80%, and when multifunctional purifying column purification, clean-up effect and the optimal (figure of the response rate
13), therefore this experimental selection 80% acetonitrile water as the Extraction solvent of this part.
The toxoflavin content (representing with peak area) that table 2 different acetonitrile volume fraction records when extracting
Remarks: ND represents and does not detects
Embodiment 5: the present embodiment in embodiment 3, have studied the supersound extraction time to extraction efficiency simultaneously to step 1
Impact.Use positive fermented maize face, using 80% acetonitrile water as Extraction solvent, have selected ultrasonic time 0min, 5min,
10min, 20min, 30min, 40min, by combining with step 2 multifunctional purifying column purification, analyze the supersound extraction time
Impact.Find to be capable of during supersound extraction 30min effective extraction of target analytes toxoflavin.Concrete outcome is shown in Table 3 institutes
Show.
The impact (representing with peak area) on toxoflavin extraction efficiency of the table 3 supersound extraction time
Embodiment 6: the present embodiment is separately added into 0.05mg/kg (Figure 14), 0.5mg/ in the fermented maize face of embodiment 2
Kg (Figure 15) and 1.5mg/kg (Figure 16) toxoflavin, and detect by same procedure, each interpolation concentration uses parallel assay 6
Part sample, investigates difference and adds the recovery of standard addition of concentration, precision and the detection limit of this method.
The response peak area obtained according to chromatography, uses external standard method, in conjunction with Fig. 1, enters toxoflavin content in sample
Row quantitative analysis, the result recorded is as shown in table 4.This method response rate is more than 78%, and precision is less than 3%.Through repeatedly weighing
Repetition measurement finds surely, and the method accuracy is high, and good stability, the detection being not less than 3 calculating the method with signal to noise ratio (S/N) is limited to
0.1mg/kg。
In table 4 fermented maize face, the different pitch-based sphere response rate and precision measure (n=6)
| Pitch-based sphere/mg/kg | Record content/mg/kg | The response rate/% | RSD/% |
| 0.1 | 0.078 | 78 | 3.5 |
| 0.5 | 0.44 | 88 | 1.9 |
| 1.5 | 1.22 | 81 | 2.3 |
Claims (3)
1. a method based on Multifunctional cleanup column-high performance liquid chromatography detection alimentary toxicosis flavin, it is characterised in that bag
Include following steps:
(1) sample extraction condition: after weighing 20～25g samples and 100mL extracting solution (80mL acetonitrile+20mL water) mixing, ultrasonic
Extracting 30min, take extracting solution, 5000r/min is centrifuged 5min, obtains supernatant.
(2) sample purification: take the supernatant 10mL that step 1 obtains, crosses Multifunctional cleanup column MycoSep226AflaZon+ and carries out
Purify；After purification, take scavenging solution 5.0mL, use N2Dry up, then with 1.0mL pure water constant volume, after vortex dissolving, obtain upper machine liquid.
(3) chromatographiccondition: upper machine liquid step 2 obtained is through being furnished with quarternary low pressure or the binary high pressure liquid of DAD detector
Phase chromatographic system carries out chromatography, chromatographic column: ODS reversed phase chromatographic column (such as ODS C18), 250*4.6mm, 5 μm；Flowing phase
For: methanol and water gradient elution, volume ratio is (0～10min, 7:93；10～20min, 98:2；20～27min, 7:93)；Enter
Sample amount: 20 μ L；Flow velocity: 1.0mL/min；Column temperature: 30 DEG C.Detection wavelength: 258nm.
(4) qualitative analysis of samples: the retention time obtained according to step 3 chromatography and characteristic light spectrogram, with the reservation of standard specimen
Time and characteristic light spectrogram are compared, if both coincide, then show containing toxoflavin.
(5) sample amounts analysis: standard specimen is prepared: toxoflavin is dissolved in water, is configured to concentration and is respectively 0.05,0.1,0.2,0.4,
1.0,2.0,5.0,10.0 μ g/mL series standards use liquid.Using standard specimen response peak area as vertical coordinate, standard specimen concentration is horizontal seat
Mark (μ g/mL), draws calibration trace.The response peak area obtained according to step 3 chromatography, uses external standard method, in sample
Toxoflavin content carries out quantitative analysis.
Method the most according to claim 1, it is characterised in that described concentration is respectively 0.05,0.1,0.2,0.4,1.0,
The compound method of 2.0,5.0,10.0 μ g/mL series standards use liquid is as follows: weighs 0.0100g toxoflavin standard substance and holds in 10ml
In measuring bottle, after methanol dissolves, it is settled to scale, is configured to 1.0mg/mL standard mother solution.It is positioned in-18 DEG C of refrigerators, Ke Yibao
Deposit 3 months.Before using, taking out and place after room temperature, take 200 μ L standard mother solutions in 10mL volumetric flask, water is settled to scale, shakes
Even, it is configured to the middle of 20.0 μ g/mL and uses liquid.Take 25 μ L, 50 μ L, 100 μ L, 200 μ L, 500 μ L, chien shih in 1.0mL respectively
With liquid and 50 μ L, 100 μ L standard mother solutions are in 10mL volumetric flask, and water is settled to scale.
Method the most according to claim 1, it is characterised in that described detection food is that frumentum fermented product (includes fermentation
Semen Maydis flour, glutinous rice flour, hang slurry cake, corn starch, vinegar bean jelly etc.), Tremella and goods thereof, potato based article is (such as Rhizoma Solani tuber osi bean noodles, sweet
Sweet potato starch, sweet potato starch etc.) etc..
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106872619A (en) * | 2017-04-24 | 2017-06-20 | 南通博泰美术图案设计有限公司 | The assay method of aflatoxin |
| CN110672769A (en) * | 2019-10-27 | 2020-01-10 | 贵州省兽药饲料监察所(贵州省兽药残留监测中心) | Method for measuring residual quantity of cantharidin yellow pigment in poultry eggs |
| CN110749689A (en) * | 2019-11-07 | 2020-02-04 | 贵州省兽药饲料监察所(贵州省兽药残留监测中心) | Method for measuring content of cantharis yellow colorant in feed |
| WO2020248317A1 (en) * | 2019-06-14 | 2020-12-17 | 深圳市疾病预防控制中心（深圳市卫生检验中心、深圳市预防医学研究所） | Hapten, artificial antigen, and antibody of toxoflavin, synthetic methods therfor and use thereof |
| WO2020248316A1 (en) * | 2019-06-14 | 2020-12-17 | 深圳市疾病预防控制中心（深圳市卫生检验中心、深圳市预防医学研究所） | Toxoflavin hapten, artificial antigen and antibody, synthesis methods therefor and applications thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106872619A (en) * | 2017-04-24 | 2017-06-20 | 南通博泰美术图案设计有限公司 | The assay method of aflatoxin |
| WO2020248317A1 (en) * | 2019-06-14 | 2020-12-17 | 深圳市疾病预防控制中心（深圳市卫生检验中心、深圳市预防医学研究所） | Hapten, artificial antigen, and antibody of toxoflavin, synthetic methods therfor and use thereof |
| WO2020248316A1 (en) * | 2019-06-14 | 2020-12-17 | 深圳市疾病预防控制中心（深圳市卫生检验中心、深圳市预防医学研究所） | Toxoflavin hapten, artificial antigen and antibody, synthesis methods therefor and applications thereof |
| CN110672769A (en) * | 2019-10-27 | 2020-01-10 | 贵州省兽药饲料监察所(贵州省兽药残留监测中心) | Method for measuring residual quantity of cantharidin yellow pigment in poultry eggs |
| CN110749689A (en) * | 2019-11-07 | 2020-02-04 | 贵州省兽药饲料监察所(贵州省兽药残留监测中心) | Method for measuring content of cantharis yellow colorant in feed |
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