CN102914607A - High performance liquid chromatography method for measuring residual amount of Fenazaquin in plant-derived food - Google Patents
High performance liquid chromatography method for measuring residual amount of Fenazaquin in plant-derived food Download PDFInfo
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Abstract
The invention provides a high performance liquid chromatography method for measuring the residual amount of Fenazaquin in a plant-derived food, and the method comprises the following steps of: vibrating and extracting a sample to be detected through acetonitrile; purifying an extraction solution through a Florisil solid phase extraction column; adopting carbon octadecyl bonded silica gel as a filling agent to carry out chromatographic column separation; and taking a moving phase has a mixed solvent of methanol and water, wherein the volume ratio of the methanol is 80-90% and the volume ratio of the water is 20-10%; the detection wavelength is 220 nm; and the column temperature is 35 DEG C. Through a comparative study of the system, the high performance liquid chromatography method for measuring the residual amount of the Fenazaquin in the plant-derived food is firstly established and has the technical characteristics of good separation effect, accuracy in measurement, high sensitivity, strong specificity, convenience and rapidness for analysis and the like.
Description
Technical field:
The present invention relates to a kind of pesticide residue analysis method, be specifically related to the high performance liquid chromatography of the fenazaquin determination of residual amount in a kind of plant-derived food.
Background technology:
Fenazaquin belongs to the quinazoline ditosylate salt acaricide, as raw material take ortho-aminobenzoic acid, make 4-hydroxyl quinazoline, again with phosphorus oxychloride reaction, the potpourri that contains 4-chloro-quinazoline hydrochloride that obtains, then 4-tert-butylbenzene alcohol reflux reaction obtains 4-(2-(4-t-butyl-phenyl) ethoxy) quinazoline hydrochloride, namely gets this product after the neutralization.Fenazaquin is mainly used on almond (almond), apple, oranges and tangerines, cotton, grape and the ornamental plant, can effectively prevent and treat true leaf mite, Panonychus citri and tetranychus telarius and purplish red short hairs mite.This compound also has bactericidal activity.China, European Union, Japan and the U.S. etc. do not formulate the maximum residue limit (MRL) of fenazaquin temporarily, the India's maximum residue limit of regulation fenazaquin in tealeaves is 3mg/kg, Korea S stipulates that its maximum residue limit in apple, spray, eggplant, grape, mandarine, pears, perilla leaf and watermelon is respectively 0.1,0.1,0.2,0.5,0.7,0.3,3 and 0.05mg/kg.
1. Food and Chemical Toxicology, 2004,42,423-428 discloses with the fenazaquin in dichloromethane extraction tealeaves and the millet paste, the florisil silica column chromatography purification, high performance liquid chromatograph is measured, and adopting acetonitrile-water=80: 20 is mobile phase.
2. " pesticide science and management, 2011,32 (8), 41-43 " discloses and used methyl alcohol: 0.05% phosphoric acid solution=the detection uv absorption was carried out the fenazaquin quantitative test at the 220nm place for mobile phase separates in 85: 15.
3. Journal of Chromatography A, 2008,1208,16-24 discloses employing hollow fiber-liquid-phase micro extraction technique and has separated 50 kinds of agricultural chemicals (containing fenazaquin) in the pick-me-up, measures with Ultra Performance Liquid Chromatography-tandem mass spectrometer.
4. Journal of Chromatography A, 2004,1036,161-169, disclose with NaOH and regulated the pH value, with the 24 kinds of novel agrochemicals residual (containing fenazaquin) in ethyl acetate-cyclohexane extraction apple jam, concentrated lemon juice, the catsup, measure with the liquid chromatography-tandem mass spectrometry instrument.
But through inventor's systematic research, the result shows that above-mentioned patent or the determined major technique condition of paper have defective in the production application of reality:
(1) selected mobile phase methanol-0.05% phosphoric acid solution of said method=85: 15 is difficult for balance at 220nm wavelength place, uses methanol-water=85: 15 o'clock instead, and peak shape, degree of separation, tailing factor and symmetry all can meet the demands.
(2) said method adopts methylene chloride as extracting solvent, and toxicity is larger, and it is larger to extract solvent load, and environmental pollution is serious, adopts acetonitrile as extracting solvent, and extraction efficiency is higher, and toxicity is little than methylene chloride.
(3) as eluting solvent, fenazaquin can not be by wash-out for said method employing normal hexane-ethyl acetate=99: 1 (V/V).
More scientific rationally for seeking for fenazaquin in the plant-derived food, have more the residue analysis method of practicality, the inventor is through the comparative study of system, provides a kind of and has been different from that above-mentioned paper or standard announce, and can be used for measuring the residual HPLC method of fenazaquin in the plant-derived food.
Summary of the invention:
Technical matters to be solved by this invention is, overcomes above-mentioned the deficiencies in the prior art, provide a kind of easy fast, and the liquid chromatogram measuring method of fenazaquin residual quantity in the low plant-derived food of cost.
The present invention for achieving the above object, the technical scheme that adopts is:
The high performance liquid chromatography of the fenazaquin determination of residual amount in a kind of plant-derived food of the present invention may further comprise the steps:
1. sample extraction:
Taking by weighing the fruit, vegetables or the grain samples 5.0-10.0g that have prepared covers in the centrifuge tube in the 50mL tool.The sample of grain class or moisture content less adds 3-5mL water, then add the 15-30mL acetonitrile, other samples directly add the 15-30mL acetonitrile, 20-60min is extracted in concussion, behind the adding 3-5g sodium chloride vortex mixing, and the centrifugal 5-15min of 5000-10000rpm, pipette the supernatant of certain volume to the heart bottle, rotary evaporation is done near, uses the n-hexane dissolution residue, and is to be clean;
2. Solid-Phase Extraction column purification
Lysate of upper step is transferred to the florisil silica solid-phase extraction column, use first the drip washing of 10-20mL normal hexane after the loading, discard efflux, use again 10-30mL normal hexane+ethyl acetate (9+1) wash-out, collect eluent in the heart bottle, rotary evaporated to dryness, residue is with methyl alcohol dissolving and constant volume, for high-performance liquid chromatogram determination;
3. chromatographic determination
Take by weighing the fenazaquin standard items, with behind methyl alcohol dissolving and the constant volume as storing solution, then further with the standard solution of methyl alcohol dilution for having concentration gradient;
Utilize liquid chromatograph that sample is detected, external standard method is quantitative;
As preferably, the efficient liquid phase chromatographic analysis condition is:
A) chromatographic column: take the carbon octadecyl silane as filling agent;
B) mobile phase: methyl alcohol+water=80+20 to 90+10 (V/V);
C) column temperature: 35 ℃;
D) flow velocity: 1mL/min;
E) sample size: 20 μ L;
F) wavelength: 220nm;
Because adopt technique scheme, beneficial effect of the present invention is:
1, set up the high performance liquid chromatography of the fenazaquin determination of residual amount in the plant-derived food (vegetables, fruit, grain), Billy is low with LC-MS/MS detection method cost, and instrument is more general, is beneficial to apply.
2, adopt the acetonitrile concussion to extract to samples such as vegetables, fruit, grains, saltout, centrifugal layering, extraction efficiency is high, and the impurity stripping is few in the extract.
3, extract adopts florisil silica Solid-Phase Extraction column purification, by the optimization to florisil silica solid-phase extraction column purification condition, has preferably clean-up effect, and guarantees that fenazaquin has the higher recovery.
4, this method has the advantages such as simple, quick, accurate, efficient, and the detection lower bound of fenazaquin is 0.02 μ g/mL, and average recovery rate is 78.0-102.0%, and the coefficient of variation (CV%) is 1.6-5.9%.This method satisfies the requirement of domestic and international relevant laws and regulations, and the technical indicators such as the recovery meet the regulation of relevant criterion.
5, the present invention can be applicable in the detection of fenazaquin residual quantity in the plant-derived product, to promoting the foreign trade of the plant-derived food of China, guarantees food security, and guarantee human body health all tool is of great significance.
Embodiment:
Below in conjunction with specific embodiment the present invention is described in further detail, but the present invention is not limited to specific embodiment.
The mensuration of fenazaquin residual quantity in embodiment 1 cucumber
1, sample extraction: take by weighing the cucumber sample 10.0g for preparing and cover in the centrifuge tube in the 50mL tool, add the 20mL acetonitrile, after 30min is extracted in concussion, add 5g sodium chloride vortex mixing, the centrifugal 10min of 8000rpm pipettes the 10mL supernatant to the heart bottle with transfer pipet, and rotary evaporation is done near in 40 ℃ of water-baths, with 2mL n-hexane dissolution residue, to be clean;
2, Solid-Phase Extraction column purification: lysate of upper step is transferred to the florisil silica solid-phase extraction column (activation of 6mL normal hexane) that has activated, use first the drip washing of 20mL normal hexane after the loading, discard efflux (coutroi velocity is no more than 2mL/mi n), use again 15mL normal hexane+ethyl acetate (9+1) wash-out, collect eluent in the heart bottle, eluent is rotary evaporated to dryness in 40 ℃ of water-baths, residue is with the methyl alcohol dissolving and be settled to 1.0mL, mixing, cross 0.45 μ m organic system filter membrane, for high-performance liquid chromatogram determination.
3, high performance liquid chromatograph is measured
According to liquid phase chromatogram condition working sample and standard operation solution, with typical curve sample solution concentration to be proofreaied and correct, external standard method is quantitative.
4, linear relationship: with the standard solution stepwise dilution, the serial mixed standard solution of five variable concentrations of preparation by concentration from low to high, is measured according to above-mentioned chromatographic condition.Each concentration determination 3 times is made canonical plotting by its concentration of standard solution Y (μ g/mL) with corresponding peak area mean value X, calculates regression equation and related coefficient, the results are shown in Table 1.
Table 1 fenazaquin series standard working fluid concentration, peak area and typical curve
5, the recovery:
Fenazaquin does not detect in the cucumber sample, adopts this cucumber sample, adds the fenazaquin standard substance of two different content levels, and each concentration is carried out 3 parallel sample, analyzes by above-mentioned chromatographic condition.Interpolation level, the recovery and coefficient of variation result of calculation see Table 2.
Add fenazaquin medicine accuracy test result (n=3) in table 2 cucumber
By table 2 result as seen: the average recovery rate of fenazaquin interpolation level is 84.7-95.7% in the cucumber, and the coefficient of variation (CV%) is 4.4-5.9%.
6, detect lower bound: add test with the cucumber blank sample, try to achieve method to the detection limit (LOD) of fenazaquin with 3 times of signal to noise ratio (S/N ratio)s.The detection lower bound of fenazaquin in the cucumber sample is 0.02mg/kg.
7, method optimizing process:
1. extract the selection of solvent: the detection of fenazaquin in the plant-derived food, removing pigment and fat is very important step.The pigment that acetonitrile extracts and the impurity of other types are less, and the solubleness of fenazaquin in acetonitrile is larger, and the extraction efficiency of acetonitrile is higher, so adopt acetonitrile as extracting solvent.
2. the selection of extracting mode: in order to increase extraction efficiency, after the vortex mixing was adopted in this experiment, concussion was extracted 30min and is extracted, and the fenazaquin in the sample can extract fully, improves extraction efficiency.
3. the selection of sample purification condition: adopt Solid-Phase Extraction (SPE) column purification technology.The florisil silica solid-phase extraction column is a kind of florisil, can adsorpting pigment and fat granule etc.Test shows selects normal hexane as sample solution, and (9: 1, V: V) as eluent, when effluent volume during greater than 15.0mL, the variation of effluent volume was not obvious on the impact of the recovery with normal hexane-ethyl acetate.
The mensuration of fenazaquin residual quantity in embodiment 2 wheats
1, sample extraction: take by weighing the wheat samples 5.0g that has prepared and cover in the centrifuge tube in the 50mL tool, add 5mL water, the 30mL acetonitrile, after 30min is extracted in concussion, add 5g sodium chloride vortex mixing, the centrifugal 10min of 8000rpm, pipette the 15mL supernatant to the heart bottle with transfer pipet, rotary evaporation is done near in 40 ℃ of water-baths, and is with 2mL n-hexane dissolution residue, to be clean;
2, Solid-Phase Extraction column purification: with example 1.
3, high performance liquid chromatograph is measured: with example 1.
4, the recovery:
Fenazaquin does not detect in the wheat samples, adopts this wheat samples, adds the fenazaquin standard solution of two different content levels, and each concentration is carried out 3 parallel sample, analyzes by above-mentioned chromatographic condition.Interpolation level, the recovery and coefficient of variation result of calculation see Table 3.
Add fenazaquin medicine accuracy test result (n=3) in table 3 wheat
By table 2 result as seen: the average recovery rate of fenazaquin interpolation level is 91.0-92.8% in the wheat, and the coefficient of variation (CV%) is 1.6-2.9%.
Claims (4)
1. the high performance liquid chromatography of the fenazaquin determination of residual amount in the plant-derived food, it is characterized in that: described assay method comprises the steps:
(1) sample is through the organic solvent mechanical shaking extraction, and extract is done near through rotary evaporation, uses the n-hexane dissolution residue, and is to be clean;
(2) adopt the Solid-Phase Extraction column purification, after organic solvent drip washing, normal hexane and ethyl acetate mixed solvent wash-out, the eluent rotary evaporation is done near, and with methyl alcohol dissolving and constant volume, high performance liquid chromatograph is measured.
2. the high performance liquid chromatography of the fenazaquin determination of residual amount in a kind of plant-derived food according to claim 1 is characterized in that, organic solvent is acetonitrile described in the step (1).
3. the high performance liquid chromatography of the fenazaquin determination of residual amount in a kind of plant-derived food according to claim 1, it is characterized in that, solid-phase extraction column is the florisil silica solid-phase extraction column described in the step (2), leacheate is normal hexane, and the normal hexane of employing and ethyl acetate mixing eluting solvent ratio are: normal hexane+ethyl acetate=9+1 (V/V).
4. the high performance liquid chromatography of the fenazaquin determination of residual amount in a kind of plant-derived food according to claim 1 is characterized in that described plant-derived food is fruit, vegetables or grain.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104374846A (en) * | 2014-11-28 | 2015-02-25 | 谱尼测试科技(天津)有限公司 | Efficient liquid chromatography of fenazaquin residue in plant-derived foods |
| CN107153101A (en) * | 2017-04-24 | 2017-09-12 | 上海市农业科学院 | A kind of detection method of plant-derived feed polyoxin |
| CN110749662A (en) * | 2018-07-22 | 2020-02-04 | 青岛谱尼测试有限公司 | Method for determining residual amount of indexazine flumioxazin in plant-derived food |
| CN116120242A (en) * | 2023-04-10 | 2023-05-16 | 佛山职业技术学院 | Quick detection device for fenazaquin in tea, and preparation and application thereof |
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2012
- 2012-11-12 CN CN 201210448914 patent/CN102914607A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104374846A (en) * | 2014-11-28 | 2015-02-25 | 谱尼测试科技(天津)有限公司 | Efficient liquid chromatography of fenazaquin residue in plant-derived foods |
| CN107153101A (en) * | 2017-04-24 | 2017-09-12 | 上海市农业科学院 | A kind of detection method of plant-derived feed polyoxin |
| CN110749662A (en) * | 2018-07-22 | 2020-02-04 | 青岛谱尼测试有限公司 | Method for determining residual amount of indexazine flumioxazin in plant-derived food |
| CN116120242A (en) * | 2023-04-10 | 2023-05-16 | 佛山职业技术学院 | Quick detection device for fenazaquin in tea, and preparation and application thereof |
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Application publication date: 20130206 |