CN104515821B - The rapid assay methods of fumonisin in a kind of corn kernel - Google Patents
The rapid assay methods of fumonisin in a kind of corn kernel Download PDFInfo
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- CN104515821B CN104515821B CN201410687392.3A CN201410687392A CN104515821B CN 104515821 B CN104515821 B CN 104515821B CN 201410687392 A CN201410687392 A CN 201410687392A CN 104515821 B CN104515821 B CN 104515821B
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Abstract
The invention discloses the rapid assay methods of fumonisin in a kind of corn kernel, belong to technical field of analysis and detection.It comprises the following steps: the extraction of fumonisin in (1) corn kernel; (2) purification of extract; (3) in corn, the analysis of fumonisin measures.The present invention can extract the fumonisin in corn more fast, more fully, to measure the content of fumonisin more accurately, significant for raising corn quality safety.
Description
Technical field
The present invention relates to technical field of analysis and detection, specifically the rapid assay methods of fumonisin in a kind of corn kernel.
Background technology
Fumonisin is a kind of secondary metabolite produced by Fusariumsp kind (mainly comprise fusarium prolifertum, intend verticillate sickle-like bacteria etc., the fumonisin of China produces primarily of intending verticillate sickle-like bacteria), and this type of metabolic product is soluble in water.The fumonisin of current discovery mainly contains 11 kinds, comprises FA1, FA2, FB1, FB2, FB3, FC1, FC2 etc., and wherein the harm of FB1 is maximum.Research finds, in corn, naturally occurring fumonisin is mainly FB1, FB2, FB3.Fumonisin just can damage to crops growth within the scope of low concentration.IARC is divided into the possible carcinogenic substance of the mankind fumonisin.Nineteen ninety, SydenhamEW etc. find that fumonisin can be carcinogenic, and may have substantial connection with the cancer of the esophagus of the mankind.Although fumonisin is less at people's body absorption, it by affecting the metabolism of sphingolipid material, and then can disturb ceramide synthesis, thus carcinogenic.Sun Guiju etc. have investigated the relation of fumonisin and mankind's cancer of the esophagus and liver cancer, and result shows that the generation of cancer of the esophagus and liver cancer and fumonisin have relation.Fumonisin has pathogenic and neurotoxicity, and horse cerebral white matter is softening, ataxia, pig pulmonary edema, hepar damnification etc. in order causing for main manifestations, even dead.Recent study finds, fumonisin also can cause child development bad.
At present, China does not also make clear stipulaties to fumonisin limit standard, and in U.S. FDA regulation corn, fumonisin maximum limit value is 2mg/kg, and in Switzerland's regulation corn, fumonisin maximum limit value is 1mg/kg.Fumonisin within the scope of low concentration just can to health exist very large threat, for this reason, FAO/WHO propose fumonisin to the threshold limit values of human body be every day intake by body weight calculate FB1, FB2, FB3 amount be no more than 2 μ g/kg.In contaminated corn, the content of fumonisin is generally lower than tens mg/kg, belongs to trace components, thus instrumental analysis etc. need be adopted to be applicable to trace, the method for trace components comes quantitatively.
Trace analysis is generally used to measure the even lower material of micrograms magnitude.In view of tested trace components can be separated by stratographic analysis well from the potpourri of complexity, be widely used in trace analysis.
At present, the detection method of fumonisin mainly chemical detection method and immunological method.Immunological method is enzyme-linked immunosorbent assay mainly; Chemical detection method comprises thin-layer chromatography, liquid chromatography, gas chromatography and LC-MS-MS etc.What present research was more is liquid chromatography and liquid chromatograph mass spectrography (LC-MS) technology.High performance liquid chromatography (HPLC) can realize qualitative and quantitative while fumonisin, but needs derivative when detecting with HPLC, detects while this is just difficult to realize multiple mycotoxin.LC-MS method has the advantage such as high sensitivity, high resolving power, and does not need to derive when detecting, and can realize the accurate qualitative and quantitative of fumonisin.
Summary of the invention
The object of the present invention is to provide the rapid assay methods of fumonisin in a kind of corn kernel, is extract based on QuEChERS and utilize UPLC/Q-TOF rapid screening to confirm fumonisin in corn kernel.The present invention is simple to operate, fast and eliminate immune affinity column or solid-phase extraction column purifying step, not only simplify experiment, and reduce cost.In addition, the present invention can extract the fumonisin in corn more fast, more fully, to measure three kinds of fumonisin content more accurately, significant for raising corn quality safety.
The technical solution adopted in the present invention is:
A rapid assay methods for fumonisin in corn kernel, is characterized in that: comprise the following steps:
(1) extraction of fumonisin in corn kernel
The corn sample taking milled, in centrifuge tube, adds extract, vortex oscillation, ultrasonic, then centrifugal after mixing,
Described extract is acetonitrile, water, glacial acetic acid volume ratio are the mixed liquor of 84:15:1;
(2) purification of corn kernel horse second of the three ten-day periods of the hot season Toxic extraction liquid
Get supernatant in purification pipe, add C18, centrifugal 5min again after vortex oscillation, collects whole supernatant, and at 45 DEG C, nitrogen blows near dry, and residue methanol/water solution is redissolved, and then crosses 0.22 μm of two-phase filter membrane, obtains solution to be measured;
In described methanol/water solution, the volume ratio of methyl alcohol and water is 5:5;
(3) detect: treat that the solution UPLC/Q – TOF to be measured that step (2) obtains measures.
Preferably, described step (1) and the middle centrifugal rotational speed of step (2) are 3000-7000r/min.
Preferably, described step (1) and the middle centrifugal rotational speed of step (2) are 5000r/min.
Preferably, described step (1) and step (2) mesoscale eddies duration of oscillation are 0.5-5min.
Preferably, described step (1) and step (2) mesoscale eddies duration of oscillation are 1min.
Preferably, comprise the following steps:
(1) extraction of fumonisin in corn kernel
The corn sample accurately taking 2.0000g milled, in 50ml centrifuge tube, adds 20ml extract, vortex oscillation 1min, ultrasonic 20min, then centrifugal 5min under the rotating speed of 5000r/min after mixing,
(2) purification of corn kernel horse second of the three ten-day periods of the hot season Toxic extraction liquid
Get 2ml supernatant in purification pipe, add 30mgC18, after vortex oscillation 1min under the rotating speed of 5000r/min centrifugal 5min, collect whole supernatant, at 45 DEG C, nitrogen blows near dry, and residue 2ml methanol/water solution is redissolved, then cross 0.22 μm of two-phase filter membrane, obtain solution to be measured;
(3) detect: treat that the solution UPLC/Q – TOF to be measured that step (2) obtains measures.
Preferably, the testing conditions of described step (3) is:
Chromatographic condition:
Chromatographic column: ThermoHypersllGOLDC18,1.9 μm, 2.1 × 100mm; Mobile phase: A phase is the 1mM ammonium acetate containing 0.1% formic acid, and B phase is methyl alcohol, gradient elution; Flow velocity: 0.3ml/min; Sample size: 2 μ L; Column temperature: 35 DEG C;
Condition of gradient elution is as follows:
0 ~ 1min, A phase is 98%;
1 ~ 2min, A are phase linear drops to 80%;
2 ~ 4.5min, A phase is 80%, keeps 2.5min;
4.5 ~ 8min, A are phase linear drops to 2%;
8 ~ 10min, A phase 2%, keeps 2min;
10 ~ 10.5min, A are phase linear rises to 98%;
10.5 ~ 12min, A phase is 98%, keeps 1.5min, balance chromatographic column.
Mass Spectrometry Conditions:
Ion gun: ESI; Detecting pattern: positive ion [M+H]
+; Taper hole voltage (Coneenergy): 40kv; Ion source temperature (Sourcetemperature): 120 DEG C; Desolventizing temperature (Desolvationgastemperature): 400 DEG C; Sweep limit M/Z:1001000; Collision energy (Collisionenergy): 4ev; Taper hole airshed (Conegasflow): 50L/h; Desolventizing airshed (Desolvationgasflow): 700L/h.
Beneficial effect of the present invention:
(1) the present invention adopts fumonisin (FB1, FB2, FB3) detection method established in conjunction with sewage sludge based on QuECHERS extracting method in corn, this method is simple to operate, fast and eliminate immune affinity column or solid-phase extraction column purifying step, not only simplify experiment, and reduce cost.Achieve the fast qualitative and quantitatively of fumonisin in corn, significant for raising corn quality safety.
(2) utilize C18 powder as cleanser, effectively can remove the materials such as starch, fats and the carbohydrate in matrix, eliminate traditional more loaded down with trivial details purifying step, it is qualitative more accurate to make.
(3) adopt acetonitrile/water/glacial acetic acid=84/15/1 acetonitrile solution as the extraction solution of fumonisin, with vortex and ultrasonic mixing extracting mode, the fumonisin in corn can be extracted more fully, more quickly.
(4) utilizing UPLC/Q-TOF accurate mass number to can be as accurate as millesimal performance makes fumonisin qualitative more accurate.
(5) adopt ThermoHypersllGOLDC18 (1.9 μm, 2.1 × 100mm) chromatographic column that isomers FB2 and FB3 can be made to divide out, it is quantitatively more accurate to make.
Accompanying drawing explanation
Accompanying drawing 1 is the recovery contrast after C18 and PSA process;
Accompanying drawing 2 is the recovery contrast after various dose C18 process;
Accompanying drawing 3 is the MS full scan figure of fumonisin (FB1, FB2, FB3) in corn;
Accompanying drawing 4 is the Selective ion mode flow graph of fumonisin (FB1, FB2, FB3) in corn;
Accompanying drawing 5 is FB in corn
1selective ion mode flow graph and mass spectrogram;
Accompanying drawing 6 is FB in corn
3selective ion mode flow graph and mass spectrogram;
Accompanying drawing 7 is FB in corn
2selective ion mode flow graph and mass spectrogram;
Accompanying drawing 8 is the Selective ion mode flow graph of positive corn sample.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples, embodiment should not regard as limiting the scope of the present invention.
1 instrument and sample
1.1 instruments:
Ultra Performance Liquid Chromatography system (ACQUITYUltraPerformanceLCWaters company) is equipped with mass spectrum (G2-QTOF time of-flight mass spectrometer Waters company), N-EVAPTM112 Nitrogen evaporator, ThermoHypersllGOLDC18 (1.9 μm, 2.1 × 100mm) chromatographic column.
1.2 samples: corn
2 methods and result
The extraction of fumonisin in 2.1 corn kernels
Accurately take the sample of 2.0000g (being accurate to 0.0001g) milled in 50ml centrifuge tube.Add 20ml extract (acetonitrile+water+glacial acetic acid=84+15+1), violent vortex oscillation 1min, ultrasonic 20min after mixing.Then centrifugal 5min under the rotating speed of 5000r/min.
The acetonitrile/water mixed solvent of high volume ratio is applicable to extracting most mycotoxin, and research shows, when solvent be acetonitrile/water and volume ratio 80/20 ~ 90/10 time, the extraction efficiency of multiple toxin all reaches higher level.Fumonisin is a kind of acidic toxins, adds the extraction efficiency that a small amount of glacial acetic acid can significantly improve fumonisin in extract.
The purification of 2.2 corn kernel horse second of the three ten-day periods of the hot season Toxic extraction liquid
Get 2ml supernatant to (containing 30mgC18) in purification pipe, after violent vortex oscillation 1min under the rotating speed of 5000r/min centrifugal 5min, collect whole supernatant, at 45 DEG C, nitrogen blows near dry.Residue 2ml methanol/water (5/5, V/V) solution redissolves, and then crosses 0.22 μm of two-phase filter membrane, obtains solution to be measured;
In order to reduce matrix effect, extend the chromatographic column life-span, need to adopt certain purification means to remove the impurity such as pigment, lipid, albumen, starch, current purification method is mainly the methods such as immune affinity column purification, Solid phase extraction and gel infiltration (GPC) purification, these methods are not only time-consuming but also cost is higher, and this just needs badly and sets up a kind of new purification method.
In recent years, (step of QuEChERS method can simply be summarized as QuEChERS (quick, easy, cheap, effective, ruggedandsafe) technology: (1) sample comminution; (2) single solvent acetonitrile extraction and isolation; (3) MgSO is added
4dewater Deng salt; (4) the adsorbent removal of impurities such as primary secondary amine (PSA) are added; (5) supernatant carries out GC-MS, LC-MS and detects) as an emerging high efficiency extraction purification techniques, be widely used in the analysis detection of residues of pesticides, its efficient, easy and green technical concept is analyzed detection field at biotoxin etc. just gradually and is applied.The cleanser comparatively commonly used in QuEChERS method mainly contains PSA and C18 etc.Find during extract purification in " 2.1 " with PSA, the fumonisin recovery very low (as Fig. 1), this may be because the amino on PSA and the carboxyl on fumonisin react, if make adsorbent with PSA also need desorb fumonisin.C18 effectively can remove the materials such as starch, fats and carbohydrate in matrix, does not also have obvious suction-operated to be studied 3 kinds of fumonisins.Therefore, experimental selection C18 is as cleanser.
The mensuration of fumonisin in 2.3 corns
FB
1, FB
2, FB
3isolation and ldentification application UPLC/Q – TOF.Adopt ThermoHypersllGOLDC18 (1.9 μm, 2.1 × 100mm) chromatographic column, column temperature 35 DEG C; Mobile phase A: 1mM ammonium acetate (containing 0.1% formic acid), Mobile phase B: methyl alcohol, gradient elution, flow velocity is 0.3mL/min, and condition of gradient elution is:
0 ~ 1min, A phase is 98%;
1 ~ 2min, A are phase linear drops to 80%;
2 ~ 4.5min, A phase is 80%, keeps 2.5min;
4.5 ~ 8min, A are phase linear drops to 2%;
8 ~ 10min, A phase 2%, keeps 2min;
10 ~ 10.5min, A are phase linear rises to 98%;
10.5 ~ 12min, A phase is 98%, keeps 1.5min, balance chromatographic column;
Sampling volume 2 μ L.
Ion gun: ESI; Detecting pattern: positive ion [M+H]
+; Taper hole voltage (Coneenergy): 40kv; Ion source temperature (Sourcetemperature): 120 DEG C; Desolventizing temperature (Desolvationgastemperature): 400 DEG C; Sweep limit M/Z:100/1000; Collision energy (Collisionenergy): 4ev; Taper hole airshed (Conegasflow): 50L/h; Desolventizing airshed (Desolvationgasflow): 700L/h.Full scan is adopted to measure three kinds of fumonisins.
According to experiment condition in 2.3, inject solution to be measured described in 2.2, carry out UPLC/Q – TOF and analyze and measure.
The full scan of fumonisin in 2.4 corn kernels
MS full scan is carried out to maize extract, as shown in Figure 3.Extract mass spectrum Selective ion mode totally 3 kinds (as Fig. 4), be respectively M/Z=722.3963 (8.66min), 706.4014 (8.86min), 706.4014 (9.03min).
FB
1go out peak at first, retention time is 8.66min (as Fig. 5), is secondly FB
3, retention time is 8.86min (as Fig. 7), and that finally go out peak is FB
2, retention time is 9.03min (as Fig. 6).
The recovery of fumonisin and matrix effect experiment in 2.5 corn kernels
Get negative corn sample, add the fumonisin mixed standard solution of three levels, process by above-mentioned experimental technique.Each Pitch-based sphere does 5 repetitions, calculates the recovery and relative standard deviation.Result (table 2) shows, and average recovery rate is 80.8% ~ 99.0%, and relative standard deviation is 1.99% ~ 3.54%.Show have good repeatability and precision.
Get not containing the corn sample of targeted fungal toxin, completely according to after above-mentioned pre-treating method process as bare substrate.In bare substrate, add certain density standard solution, then go up machine testing, make matrix matching typical curve.This research adopts SSE (SignalSuppression/Enhancement) to evaluate matrix effect.
Result shows, and SSE, about 110%, shows do not have obvious matrix effect.Show to adopt the fumonisin in the method examination confirmation corn can meet daily demand.
Table 1 fumonisin structural formula and parent ion theoretical value
Table 2FB
1, FB
2, FB
3the method recovery and precision (n=5)
Claims (6)
1. the rapid assay methods of fumonisin in corn kernel, is characterized in that, comprise the following steps:
(1) extraction of fumonisin in corn kernel
The corn sample taking milled, in centrifuge tube, adds extract, vortex oscillation, and ultrasonic, then centrifugal after mixing, described extract is acetonitrile, water, glacial acetic acid volume ratio are the mixed liquor of 84:15:1;
(2) purification of corn kernel horse second of the three ten-day periods of the hot season Toxic extraction liquid
Get supernatant in purification pipe, add C18, centrifugal 5min again after vortex oscillation, collects whole supernatant, and at 45 DEG C, nitrogen blows near dry, and residue methanol/water solution is redissolved, and then crosses 0.22 μm of two-phase filter membrane, obtains solution to be measured;
In described methanol/water solution, the volume ratio of methyl alcohol and water is 5:5;
(3) detect: treat that the solution UPLC/Q – TOF to be measured that step (2) obtains measures;
The testing conditions of described step (3) is:
Chromatographic condition:
Chromatographic column: ThermoHypersllGOLDC18,1.9 μm, 2.1 × 100mm; Mobile phase: A phase is the 1mM ammonium acetate containing 0.1% formic acid, and B phase is methyl alcohol, gradient elution; Flow velocity: 0.3ml/min; Sample size: 2 μ L; Column temperature: 35 DEG C;
Condition of gradient elution is as follows:
0 ~ 1min, A phase is 98%;
1 ~ 2min, A are phase linear drops to 80%;
2 ~ 4.5min, A phase is 80%, keeps 2.5min;
4.5 ~ 8min, A are phase linear drops to 2%;
8 ~ 10min, A phase 2%, keeps 2min;
10 ~ 10.5min, A are phase linear rises to 98%;
10.5 ~ 12min, A phase is 98%, keeps 1.5min, balance chromatographic column;
Mass Spectrometry Conditions:
Ion gun: ESI; Detecting pattern: positive ion [M+H]
+; Taper hole voltage: 40kv; Ion source temperature: 120 DEG C; Desolventizing temperature: 400 DEG C; Sweep limit M/Z:100/1000; Collision energy: 4ev; Taper hole airshed: 50L/h; Desolventizing airshed: 700L/h.
2. the rapid assay methods of fumonisin in a kind of corn kernel according to claim 1, is characterized in that, in described step (1) and step (2), centrifugal rotational speed is 3000-7000r/min.
3. the rapid assay methods of fumonisin in a kind of corn kernel according to claim 2, is characterized in that, in described step (1) and step (2), centrifugal rotational speed is 5000r/min.
4. the rapid assay methods of fumonisin in a kind of corn kernel according to claim 1, it is characterized in that, described step (1) and step (2) mesoscale eddies duration of oscillation are 0.5-5min.
5. the rapid assay methods of fumonisin in a kind of corn kernel according to claim 4, it is characterized in that, described step (1) and step (2) mesoscale eddies duration of oscillation are 1min.
6., according to the rapid assay methods of fumonisin in the arbitrary described a kind of corn kernel of claim 1-5, it is characterized in that, comprise the following steps:
(1) extraction of fumonisin in corn kernel
The corn sample accurately taking 2.0000g milled, in 50ml centrifuge tube, adds 20ml extract, vortex oscillation 1min, ultrasonic 20min, then centrifugal 5min under the rotating speed of 5000r/min after mixing,
(2) purification of corn kernel horse second of the three ten-day periods of the hot season Toxic extraction liquid
Get 2ml supernatant in purification pipe, add 30mgC18, after vortex oscillation 1min under the rotating speed of 5000r/min centrifugal 5min, collect whole supernatant, at 45 DEG C, nitrogen blows near dry, and residue 2ml methanol/water solution is redissolved, then cross 0.22 μm of two-phase filter membrane, obtain solution to be measured;
(3) detect: treat that the solution UPLC/Q – TOF to be measured that step (2) obtains measures.
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| CN104931308B (en) * | 2015-05-18 | 2018-02-06 | 上海市农业科学院 | A kind of method for preparing fumonisin B1, B2 and B3 standard items simultaneously |
| CN106248837B (en) * | 2016-10-08 | 2019-10-01 | 江苏省农业科学院 | The Liquid Chromatography-Tandem Mass Spectrometry detection method of fumonisin in a kind of cereal |
| CN106442817A (en) * | 2016-11-30 | 2017-02-22 | 无锡艾科瑞思产品设计与研究有限公司 | Method for detecting mold in food |
| CN107192756A (en) * | 2017-04-27 | 2017-09-22 | 哈尔滨市农产品质量安全检验检测中心 | The detection means of a variety of mycotoxins in a kind of on-line checking corn |
| CN110007042A (en) * | 2019-04-25 | 2019-07-12 | 江苏省农业科学院 | The detection method of cereal fumonisin and its derivative |
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