CN104977383A - Method for rapidly and quantitatively detecting microcystins in spirulina food - Google Patents
Method for rapidly and quantitatively detecting microcystins in spirulina food Download PDFInfo
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Abstract
The invention relates to a method for rapidly and quantitatively detecting microcystins in a spirulina food. The detection method comprises the following steps: taking a proper amount of a spirulina solid sample, and preprocessing to obtain a sample solution to be detected; adding ultrapure water to microcystin RR and microcystin LR standard substances to prepare positive control solutions; adding the prepared sample solution to be detected into an HLB column, enriching, eluting, centrifuging, and taking the obtained supernatant to be detected; and carrying out HPLC-tandem mass spectrometry determination on the supernatant to be detected. In the invention, acetate acid gracial or an aqueous solution containing butanol and methanol according to a specific volume ratio is adopted as an extract liquid, so the extracting recovery rate is high; and mass spectrometric multi-reaction monitoring is adopted, and chromatographic conditions and mass spectrometric parameters are maximally optimized, so interferences are effectively overcome, the selectivity and the sensitivity are high, the analysis time is short, and rapid detection of microcystins in the spirulina food by a quality supervision department can be met.
Description
Technical field
The invention belongs to field of food detection, be specifically related to the fast quantitative measurement method for detecting of micro-capsule toxin in a kind of spirulina based food.
Background technology
Edible algae main at present mainly contains spirulina and chlorella.Spiral algae contains abundant nutritional labeling, comprises multivitamin (B1, B2, B6, B12, C, E, K etc.), mineral matter (calcium, iron, zinc, phosphorus, magnesium and iodine etc.), amino acid, beta carotene, gamma-linoleic acid, chlorophyll and protein.The World Health Organization (WHO) (WHO) is decided to be " optimum medicines of mankind's 21 century ", U.S. foods in 1981 and drug administration (FDA) confirm as " one of optimum protein matter source ", and the Ministry of Public Health of China also ratifies it for " new resource food "., at present, spirulina was carried out to the Toxicological evaluation of system both at home and abroad, confirms that it is the food of safe and effective health.Along with the raising of living standards of the people and health care consciousness, the demand of people to health food is increasing, it is also proposed higher requirement to health food security simultaneously.And spirulina is being propagated artificially with in physical environment, all may be polluted by poisonous blue-green algae, can there is the Microcystin of infringement in association one class to human liver.Microcystin is a kind of monocycle 7 peptide, isomers to 21 beginning of the century fixed MCYSTs has reached kind more than 60, it is the class algae toxin that the frequency of occurrences is the highest, product poison amount is maximum in blue-green alga bloom pollutes, it has strong tumor promotion, the target organ of its effect is liver, it can the activity of Profilin phosphatase consumingly, causes the peroxophosphoric acid of multiple proteins in cell, causes hepatocellular damage.Due to its ecotoxicological effect, day by day cause the concern of people.In recent years, because global environmental pollution increases the weight of, expose by the water body producing malicious Microcystis aeruginosa and other harmful blue-green algae pollution the public health problem that Microcystin is facing mankind.Some countries and WHO also recommend the threshold limit values standard of Microcystin in potable water and recreational water, and therefore, the content how effectively detecting the Microcystin be mixed in spirulina is most important for the quality monitoring of China to algae health products.
At present, the detection method of Microcystin comprises phosphoprotein phosphatase inhibition analysis PPIA method, ELISA method and HPLC method, and PPIA method, ELISA method are easily disturbed in testing process, and in HPLC method testing process, sample pre-treatments is complicated.For this reason, the invention provides a kind of detection sensitivity high, quantitatively Ultra Performance Liquid Chromatography-serial connection Mass Spectrometry detection method accurately.
Summary of the invention
The object of the invention is to solve the above-mentioned problems in the prior art, provide that a kind of detection sensitivity is high, strong interference immunity and the testing result detection method of micro-capsule toxin in spirulina based food accurately.
Technical scheme of the present invention is as follows:
A fast quantitative measurement method for detecting for micro-capsule toxin in spirulina based food, comprises the following steps:
(1) sample pre-treatments: get spirulina solid sample 1-5g, be placed in grind after alms bowl grinds and add Extraction solvent, put into magnetic stirring apparatus to blend, centrifugal, use GF/C Filter paper filtering after precipitation, again add extract, repeat to extract 3-5 time, extract is placed in and Rotary Evaporators is heated concentrated, obtain sample liquid to be measured for subsequent use;
(2) prepare positive control solution: get micro-capsule toxin RR and micro-capsule toxin LR standard items 1-5g, add ultrapure water and dissolve that to be mixed with the positive control solution of 1.0ug/ml for subsequent use;
(3) sample purification: the sample liquid to be measured of preparation in step (1) is added in HLB post and carries out enrichment, wash-out, collects eluent and is placed in flask, evaporate to dryness on Rotary Evaporators, enrichment again, wash-out again, and by eluent evaporate to dryness on Rotary Evaporators, get the methyl alcohol that the sample after evaporate to dryness adds 3-5 times of volume, proceed in centrifuge tube, add 5-10ml purified water to dissolve, centrifugal, get supernatant to be measured;
(4) content of micro-capsule toxin in HPLC working sample: the positive control solution of the 1.0ug/ml prepared in step (2) is carried out respectively one-level full scan and the many reaction detection of secondary full scan machine, optimize chromatographic condition and Mass Spectrometry Conditions, HPLC-is carried out to the supernatant to be measured in step (3) and is connected in series mass spectrometric determination.
Preferably, the spirulina solid sample formulation described in step (1) comprises capsule, tablet and fine powder.
Preferably, the addition of the Extraction solvent described in step (1) is 30-50ml.
Preferably, the Extraction solvent described in step (1) is selected from one or more in glacial acetic acid or alcoholic solution.
Preferably, the glacial acetic acid of to be volumetric concentration the be 5-10% of the glacial acetic acid described in step (1).
Preferably, the alcoholic solution described in step (1) is the mixed solution of butanols, first alcohol and water, and the volume ratio of described butanols, methyl alcohol, water is (1-3): (4-12): (20-50).
Preferably, step (1) and the centrifugal speed described in step (3) are 10000-12000r/min, and centrifugation time is 20-30min; Warm temperature described in step (1) is 50-80 DEG C.
Preferably, the elution process described in step (3) is specially: the methanol aqueous solution wash-out first using 20-30%, then the methanol aqueous solution wash-out using 90-100%.
Preferably, in step (3), elution process is specially again: the methanol aqueous solution wash-out by concentration being first 10-20%, then uses the methanol aqueous solution wash-out of 60-70%.
Preferably, the chromatographic condition in step (4) is: mobile phase is the potpourri of 0.3 % aqueous formic acid and acetonitrile, and wherein the volume ratio of 0.3 % aqueous formic acid and acetonitrile 2-5 is (1-3): (2-5); Flow velocity: 0.4 mL/min; Chromatographic column: Waters Acquity UPLC TM BEH C 18,1.7 μm, 2.1 mm × 100 mm; Column temperature: 40-45 DEG C; Sample disc temperature: 4 DEG C; Elution program: degree of grade, the 0.3 % aqueous formic acid of 80 %, 20 % acetonitriles; Sample size: 5 μ L; Mass Spectrometry Conditions: instrument: Agilent 6460 type triple quadrupole mass spectrometer; Ionization source pattern: electro-spray ionization; Ionization source polarity: positive ion mode; Atomization gas: nitrogen; Atomization gas pressure: 50-55psi; Capillary voltage: 3400-3600V; Dry gas temperature: 325-340 DEG C; Dry gas flow velocity: 5 L/min; Sheath temperature degree: 380-400 DEG C; Sheath gas velocity: 12 L/min; Monitoring mode: multiple-reaction monitoring.
Compared with prior art, beneficial effect is embodied in the present invention:
1. in the testing process of micro-capsule toxin, conventional extract [methyl alcohol, acidified methanol (0.05 % TFA), EDTA Na
2(0.01 mol/L)-acidified methanol (0.05 % TFA)] although extract target component effect, because its component is too complicated, easily produce matrix effect, affect the quantitative test of later stage target component.In the present invention, adopting volumetric concentration to be the glacial acetic acid of 5-10% or volume ratio is (1-3): (4-12): the butanols of (20-50), the aqueous solution of methyl alcohol are as extract, the higher recovery can be obtained when extraction two kinds of micro-capsule toxin, effectively can improve the extraction of target components.
2. current, the assay method of Microcystins comprises many, and the assay method of Microcystin is comparatively ripe in water sample, and the study on determination method of micro-capsule toxin few in biological sample and spiral algae solid sample, and foreign scholar etc. adopt immune affinity column purifying HPLC to detect, sample recovery of standard addition is about 80%.This research, traditional assay method basis adopts mass spectrum multiple-reaction monitoring, effectively can overcome and detect in sample interfering component to the impact of testing result, and by measuring the fragment ion peak of specific mass-to-charge ratio, selectivity and sensitivity is all higher.
3. because interfering component in spirulina based food is more, in order to improve peak shape, improving sample separation degree, shortening analysis time, in the present invention when carrying out pre-service to sample, adopt twice gradient elution, in HPLC-tandem mass spectrum testing process, also select gradient elution, outflow Component seperation Du Genggao can be made, and the peak symmetry of chromatographic peak can be significantly improved, make target component separating effect better, avoid the impact that endogenous impurity is separated target component.
4. this research is in employing mass spectrum multiple-reaction monitoring process, and the aqueous formic acid of the designated volume ratio of selection certain concentration and acetonitrile, as mobile phase, can significantly improve the Ionization Efficiency of micro-capsule toxin RR and micro-capsule toxin LR sample and detect response sensitivity.
5. in order to obtain the best mass spectrometry parameters of micro-capsule Mycotoxin identification, the present invention is also provided with positive controls, has all carried out maximum optimization, thus improve the sensitivity of detection and the accuracy of testing result to greatest extent to chromatographic condition and mass spectrometry parameters.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail:
Described positive reference substance micro-capsule toxin RR and micro-capsule toxin LR standard items are purchased from TaiWan Algal Science Inc.
Embodiment 1
A fast quantitative measurement method for detecting for micro-capsule toxin in spirulina based food, comprises the following steps:
(1) sample pre-treatments: get spirulina capsule sample 1g, be placed in the glacial acetic acid grinding and add 30ml 5% after alms bowl grinds, put into magnetic stirring apparatus to blend, with the centrifugal 20min of 10000r/min, use GF/C Filter paper filtering after precipitation, again add extract, repeat extraction 3 times, being placed in by extract Rotary Evaporators heats to 50 DEG C concentrates, and obtains sample liquid to be measured for subsequent use;
(2) prepare positive control solution: get micro-capsule toxin RR and micro-capsule toxin LR standard items 1g, add ultrapure water and dissolve that to be mixed with the positive control solution of 1.0ug/ml for subsequent use;
(3) sample purification: the sample liquid to be measured of preparation in step (1) is added in HLB post and carries out enrichment, first use the methanol aqueous solution wash-out of 20%, use the methanol aqueous solution wash-out of 90% again, collect eluent and be placed in flask, evaporate to dryness on Rotary Evaporators, enrichment again, again with 10% methanol aqueous solution wash-out, use the methanol aqueous solution wash-out wash-out of 60% again, and by eluent evaporate to dryness on Rotary Evaporators, get the methyl alcohol that the sample after evaporate to dryness adds 3 times of volumes, proceed in centrifuge tube, add 5ml purified water to dissolve, with the centrifugal 20min of 10000r/min, get supernatant to be measured,
(4) content of micro-capsule toxin in HPLC working sample: the positive control solution of the 1.0ug/ml prepared in step (2) is carried out respectively one-level full scan and the many reaction detection of secondary full scan machine, optimize chromatographic condition and Mass Spectrometry Conditions, HPLC-is carried out to the supernatant to be measured in step (3) and is connected in series mass spectrometric determination.
Chromatographic condition in step (4) is: mobile phase is the potpourri of 0.3 % aqueous formic acid 1 parts by volume and acetonitrile 2 parts by volume; Flow velocity: 0.4 mL/min; Chromatographic column: Waters Acquity UPLC TM BEH C 18,1.7 μm, 2.1 mm × 100 mm; Column temperature: 40 DEG C; Sample disc temperature: 4 DEG C; Elution program: degree of grade, the 0.3 % aqueous formic acid of 80 %, 20 % acetonitriles; Sample size: 5 μ L; Mass Spectrometry Conditions: instrument: Agilent 6460 type triple quadrupole mass spectrometer; Ionization source pattern: electro-spray ionization; Ionization source polarity: positive ion mode; Atomization gas: nitrogen; Atomization gas pressure: 50psi; Capillary voltage: 3400 V; Dry gas temperature: 325 DEG C; Dry gas flow velocity: 5 L/min; Sheath temperature degree: 380 DEG C; Sheath gas velocity: 12 L/min; Monitoring mode: multiple-reaction monitoring.
Embodiment 2
A fast quantitative measurement method for detecting for micro-capsule toxin in spirulina based food, comprises the following steps:
(1) sample pre-treatments: get spirulina tablet sample 5g, be placed in the solution grinding and add butanols that 50ml volume ratio is 1:4:20, methyl alcohol, water after alms bowl grinds, put into magnetic stirring apparatus to blend, with the centrifugal 30min of 12000r/min, use GF/C Filter paper filtering after precipitation, again add extract, repeat extraction 5 times, being placed in by extract Rotary Evaporators heats to 80 DEG C concentrates, and obtains sample liquid to be measured for subsequent use;
(2) prepare positive control solution: get micro-capsule toxin RR and micro-capsule toxin LR standard items 1-5g, add ultrapure water and dissolve that to be mixed with the positive control solution of 1.0ug/ml for subsequent use;
(3) sample purification: the sample liquid to be measured of preparation in step (1) is added in HLB post and carries out enrichment, first use the methanol aqueous solution wash-out of 30%, use the methanol-eluted fractions of 100% again, collect eluent and be placed in flask, evaporate to dryness on Rotary Evaporators, enrichment again, again first with the methanol aqueous solution wash-out that concentration is 20%, use the methanol aqueous solution wash-out wash-out of 70% again, and by eluent evaporate to dryness on Rotary Evaporators, get the methyl alcohol that the sample after evaporate to dryness adds 5 times of volumes, proceed in centrifuge tube, add 10ml purified water to dissolve, with the centrifugal 30min of 12000r/min, get supernatant to be measured,
(4) content of micro-capsule toxin in HPLC working sample: the positive control solution of the 1.0ug/ml prepared in step (2) is carried out respectively one-level full scan and the many reaction detection of secondary full scan machine, optimize chromatographic condition and Mass Spectrometry Conditions, HPLC-is carried out to the supernatant to be measured in step (3) and is connected in series mass spectrometric determination.
Preferably, the chromatographic condition in step (4) is: mobile phase is the potpourri of 0.3 % aqueous formic acid 3 parts by volume and acetonitrile 5 parts by volume; Flow velocity: 0.4 mL/min; Chromatographic column: Waters Acquity UPLC TM BEH C 18,1.7 μm, 2.1 mm × 100 mm; Column temperature: 45 DEG C; Sample disc temperature: 4 DEG C; Elution program: degree of grade, the 0.3 % aqueous formic acid of 80 %, 20 % acetonitriles; Sample size: 5 μ L; Mass Spectrometry Conditions: instrument: Agilent 6460 type triple quadrupole mass spectrometer; Ionization source pattern: electro-spray ionization; Ionization source polarity: positive ion mode; Atomization gas: nitrogen; Atomization gas pressure: 55psi; Capillary voltage: 3600V; Dry gas temperature: 340 DEG C; Dry gas flow velocity: 5 L/min; Sheath temperature degree: 400 DEG C; Sheath gas velocity: 12 L/min; Monitoring mode: multiple-reaction monitoring.
Embodiment 3
A fast quantitative measurement method for detecting for micro-capsule toxin in spirulina based food, comprises the following steps:
(1) sample pre-treatments: get spirulina fine powder sample 3g, be placed in the solution grinding and add butanols that 40ml volume ratio is 3:12:50, methyl alcohol, water after alms bowl grinds, put into magnetic stirring apparatus to blend, with the centrifugal 25min of 11000r/min, use GF/C Filter paper filtering after precipitation, again add extract, repeat extraction 4 times, being placed in by extract Rotary Evaporators heats to 60 DEG C concentrates, and obtains sample liquid to be measured for subsequent use;
(2) prepare positive control solution: get micro-capsule toxin RR and micro-capsule toxin LR standard items 3g, add ultrapure water and dissolve that to be mixed with the positive control solution of 1.0ug/ml for subsequent use;
(3) sample purification: the sample liquid to be measured of preparation in step (1) is added in HLB post and carries out enrichment, first use the methanol aqueous solution wash-out of 25%, use the methanol aqueous solution wash-out of 95% again, collect eluent and be placed in flask, evaporate to dryness on Rotary Evaporators, enrichment again, again with 15% methanol aqueous solution wash-out, use the methanol aqueous solution wash-out of 65% again, and by eluent evaporate to dryness on Rotary Evaporators, get the methyl alcohol that the sample after evaporate to dryness adds 4 times of volumes, proceed in centrifuge tube, add 8ml purified water to dissolve, with the centrifugal 25min of 11000r/min, get supernatant to be measured,
(4) content of micro-capsule toxin in HPLC working sample: the positive control solution of the 1.0ug/ml prepared in step (2) is carried out respectively one-level full scan and the many reaction detection of secondary full scan machine, optimize chromatographic condition and Mass Spectrometry Conditions, HPLC-is carried out to the supernatant to be measured in step (3) and is connected in series mass spectrometric determination.
Preferably, the chromatographic condition in step (4) is: mobile phase: the potpourri of 0.3 % aqueous formic acid 2 parts by volume and acetonitrile 3 parts by volume; Flow velocity: 0.4 mL/min; Chromatographic column: Waters Acquity UPLC TM BEH C 18,1.7 μm, 2.1 mm × 100 mm; Column temperature: 42 DEG C; Sample disc temperature: 4 DEG C; Elution program: degree of grade, the 0.3 % aqueous formic acid of 80 %, 20 % acetonitriles; Sample size: 5 μ L; Mass Spectrometry Conditions: instrument: Agilent 6460 type triple quadrupole mass spectrometer; Ionization source pattern: electro-spray ionization; Ionization source polarity: positive ion mode; Atomization gas: nitrogen; Atomization gas pressure: 52psi; Capillary voltage: 3500V; Dry gas temperature: 330 DEG C; Dry gas flow velocity: 5 L/min; Sheath temperature degree: 390 DEG C; Sheath gas velocity: 12 L/min; Monitoring mode: multiple-reaction monitoring.
Above-described embodiment is only the preferred embodiment of the present invention, and should not be construed as limitation of the invention, and those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (10)
1. the fast quantitative measurement method for detecting of micro-capsule toxin in spirulina based food, is characterized in that, comprise the following steps:
(1) sample pre-treatments: get spirulina solid sample 1-5g, be placed in grind after alms bowl grinds and add Extraction solvent, put into magnetic stirring apparatus to blend, centrifugal, use GF/C Filter paper filtering after precipitation, again add extract, repeat to extract 3-5 time, extract is placed in and Rotary Evaporators is heated concentrated, obtain sample liquid to be measured for subsequent use;
(2) prepare positive control solution: get micro-capsule toxin RR and micro-capsule toxin LR standard items 1-5g, add ultrapure water and dissolve that to be mixed with the positive control solution of 1.0ug/ml for subsequent use;
(3) sample purification: the sample liquid to be measured of preparation in step (1) is added in HLB post and carries out enrichment, wash-out, collects eluent and is placed in flask, evaporate to dryness on Rotary Evaporators, enrichment again, wash-out again, and by eluent evaporate to dryness on Rotary Evaporators, get the methyl alcohol that the sample after evaporate to dryness adds 3-5 times of volume, proceed in centrifuge tube, add 5-10ml purified water to dissolve, centrifugal, get supernatant to be measured;
(4) HPLC-is connected in series the content of micro-capsule toxin in mass spectrometric determination sample: the positive control solution of the 1.0ug/ml prepared in step (2) is carried out respectively one-level full scan and the many reaction detection of secondary full scan machine, optimize chromatographic condition and Mass Spectrometry Conditions, HPLC-is carried out to the supernatant to be measured in step (3) and is connected in series mass spectrometric determination.
2. the fast quantitative measurement method for detecting of micro-capsule toxin in a kind of spirulina based food according to claim 1, is characterized in that, the spirulina solid sample formulation described in step (1) be selected from capsule, tablet or fine powder one or more.
3. the fast quantitative measurement method for detecting of micro-capsule toxin in a kind of spirulina based food according to claim 1, it is characterized in that, the addition of the Extraction solvent described in step (1) is 30-50ml.
4. the fast quantitative measurement method for detecting of micro-capsule toxin in a kind of spirulina based food according to claim 1, is characterized in that, the Extraction solvent described in step (1) be selected from glacial acetic acid or alcoholic solution one or more.
5. the fast quantitative measurement method for detecting of micro-capsule toxin in a kind of spirulina based food according to claim 4, is characterized in that, the glacial acetic acid of to be volumetric concentration the be 5-10% of the glacial acetic acid described in step (1).
6. the fast quantitative measurement method for detecting of micro-capsule toxin in a kind of spirulina based food according to claim 4, it is characterized in that, alcoholic solution described in step (1) is the mixed solution of butanols, methyl alcohol, water, preferably, the volume ratio of described butanols, first alcohol and water is (1-3): (4-12): (20-50).
7. the fast quantitative measurement method for detecting of micro-capsule toxin in a kind of spirulina based food according to claim 1, is characterized in that, step (1) and the centrifugal speed described in step (3) are 10000-12000r/min, and centrifugation time is 20-30min; Warm temperature described in step (1) is 50-80 DEG C.
8. the fast quantitative measurement method for detecting of micro-capsule toxin in a kind of spirulina based food according to claim 1, it is characterized in that, elution process described in step (3) is specially: the methanol aqueous solution wash-out first using 20-30%, then the methanol aqueous solution wash-out using 90-100%.
9. the fast quantitative measurement method for detecting of micro-capsule toxin in a kind of spirulina based food according to claim 1, it is characterized in that, in step (3), elution process is specially again: the methanol aqueous solution wash-out by concentration being first 10-20%, then uses the methanol aqueous solution wash-out of 60-70%.
10. the fast quantitative measurement method for detecting of micro-capsule toxin in a kind of spirulina based food according to claim 1, it is characterized in that, chromatographic condition in step (4) is: mobile phase is the potpourri of 0.3 % aqueous formic acid and acetonitrile, and wherein the volume ratio of 0.3 % aqueous formic acid and acetonitrile 2-5 is (1-3): (2-5); Flow velocity is 0.4 mL/min; Chromatographic column: Waters Acquity UPLC TM BEH C 18,1.7 μm, 2.1 mm × 100 mm; Column temperature: 40-45 DEG C; Sample disc temperature: 4 DEG C; Elution program: degree of grade, the 0.3 % aqueous formic acid of 80 %, 20 % acetonitriles; Sample size: 5 μ L; Mass Spectrometry Conditions: instrument: Agilent 6460 type triple quadrupole mass spectrometer; Ionization source pattern: electro-spray ionization; Ionization source polarity: positive ion mode; Atomization gas: nitrogen; Atomization gas pressure: 50-55psi; Capillary voltage: 3400-3600V; Dry gas temperature: 325-340 DEG C; Dry gas flow velocity: 5 L/min; Sheath temperature degree: 380-400 DEG C; Sheath gas velocity: 12 L/min; Monitoring mode: multiple-reaction monitoring.
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Application publication date: 20151014 |