CN101799460B - Method for detecting organophosphorus pesticide residue in tobacco - Google Patents
Method for detecting organophosphorus pesticide residue in tobacco Download PDFInfo
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Abstract
The invention discloses a method for detecting the organophosphorus pesticide residue in the tobacco, comprising the following steps of preprocessing by adding water of 5-15 times the weight of the tobacco sample to the tobacco sample to sock the tobacco sample, adding 10-20 ml of extracting agent to each gram of the tobacco sample to extract the tobacco sample, centrifuging to obtain organic-phase supernatant, purifying the organic-phase supernatant, concentrating the organic-phase supernatant by blowing with nitrogen, adding acetone solution to the organic-phase supernatant, and filtering the organic-phase supernatant with a organic-phase filtering membrane of 0.2 Mum to obtain the sample solution, wherein the extracting agent is the mixed solution of acetonitrile and acetone which are at the volume ratio of 1-2:1; and detecting the organophosphorus pesticide residue in the sample solution with gas chromatography and mass spectroscopy by using the chlorazol phosphorus as the internal standard substance after finishing preprocessing. Because the extracting agent is used for extracting in the preprocessing step, the target substance in the tobacco sample can be effectively extracted into the organic phase, and the precision for detecting the organophosphorus pesticide residue in the tobacco can be greatly improved.
Description
Technical field
The present invention relates to one grow tobacco in the method for quick of organophosphorus pesticide residual quantity, belong to the trace analysis technical field.
Background technology
In the plantation of tobacco, storage process, can produce big residues of pesticides, wherein organophosphorus pesticide (OPs) wide in variety, active wide, drug effect is high, be widely used.Because the unstable chemcial property of these organophosphorus pesticides, than being easier to oxidation, hydrolysis etc., tend in vivo be oxidized to than the higher compound of agricultural chemicals substance toxicity, so these residues of pesticides are present in the middle of the tobacco, and then can cause huge harm to the health of human body.Therefore no matter from tobacco and tobacco product security standpoint or environmental protection angle, organophosphorus pesticide all has very important significance in the detection tobacco.At present the research of agricultural chemicals residue analysis method also is one of analytical chemistry field hot issue in tobacco and the tobacco product, and method is effectively simple and to cover more detected objects are development trends that organophosphorus pesticide is analyzed in the tobacco in recent years.
When the detection of residues of pesticides, the processing of tobacco sample influences the principal element of detection efficiency often, because the complicacy of tobacco sample itself, a lot of pre-treating methods or can only be at independent or a small amount of analytic target, perhaps pre-treatment step is too loaded down with trivial details, operation easier is big, the reagent consumption height, and extraction efficiency is difficult to improve.Detect the method for organophosphorus pesticide in tobacco and the tobacco product such as existing GB/T 13595-2004, its pre-treatment process more complicated, not only need through steps such as liquid-liquid extraction, gel permeation chromatography purification, silica gel column chromatography column purifications, only the organic solvent of Shi Yonging is just above 6 kinds; And loss or the destruction that in the pre-treatment process, also can cause analytic target, influence final testing result.
Summary of the invention
The method that the purpose of this invention is to provide organophosphorus pesticide residual quantity in a kind of accurate detection tobacco.
In order to realize above purpose, the technical solution adopted in the present invention is: a kind of method that detects organophosphorus pesticide residual quantity in the tobacco, comprise following sample pre-treatments: add tobacco sample weight 5-15 water logging bubble doubly, the extractant that adds every gram tobacco sample 10-20ml again extracts, carrying out centrifuging and taking part upper organic phase clear liquid after the extraction brushes concentrated through purified treatment, nitrogen, add acetone soln then, obtain sample solution through 0.22 μ m organic phase membrane filtration; Wherein extractant is the mixed liquor of acetonitrile and acetone, and the volume ratio of acetonitrile and acetone is 1-2:1; After the pre-treatment, be that internal standard compound adopts the organophosphorus pesticide residual quantity in the gaschromatographic mass spectrometry method test sample solution with the isazofos with the sample solution that obtains.
Described organophosphorus pesticide is: DDVP, Menite, orthene, thionazin, terbufos, disulfoton, iprobenfos, phosphamidon, chlorpyrifos-methyl, Nankor, tolelofos-methyl, parathion-methyl, formothion, fenifrothion, ethyl parathion, ethyl-pyrimidine phosphorus, bromophos, Rilariol, chlorine third phosphorus, azinphos-methyl.
Also add anhydrous magnesium sulfate and the sodium chloride that saturating capacity is arranged during described extraction.
Described purified treatment is: the upper organic phase clear liquid after centrifugal is inserted in the container with PSA adsorbent and anhydrous magnesium sulfate, and centrifugal treating is carried out in shaking again.
Method of the present invention specifically comprises the steps:
1) preparation of mixed standard solution: get the mixed standard solution that each organophosphorus pesticide standard items is blended at least three concentration of preparation in the 0.01-1 μ g/ml concentration range, add the internal standard compound isazofos during preparation, the concentration of isazofos in each mixed standard solution is 0.5 μ g/ml;
2) pre-treatment of sample: accurately take by weighing the dry sample after the pulverizing, place centrifuge tube, add example weight 5-15 ultrapure water doubly and soak 20min, add acetonitrile, anhydrous magnesium sulfate, sodium chloride and acetone then, jolting 2min immediately is in the centrifugal 10min of 7000 rpm; Getting above-mentioned upper organic phase clear liquid after centrifugal joins in the centrifuge tube that is placed with PSA adsorbent and anhydrous magnesium sulfate, jolting 30s, in the centrifugal 10min of 10000 rpm, draw supernatant liquor in the nitrogen bottle blowing, blow down concentrated at 40 ℃ of water-bath nitrogen, add acetone soln again, through 0.22 μ m organic phase membrane filtration;
3) gaschromatographic mass spectrometric analysis:
Analytical conditions for gas chromatography:
Chromatographic column: DB-17MS elastic quartz capillary tube chromatographic column (30m * 0.32mm * 0.25 μ m);
Injector temperature: 270 ℃;
Temperature programme: 70 ℃ of initial temperatures keep 1min after keeping behind the 1min being raised to 150 ℃ with 15 ℃/min; Be raised to 190 ℃ with 1 ℃/min then, be raised to 270 ℃ with 15 ℃/min at last, keep 10min;
Input mode: split sampling not;
Carrier gas: helium, constant current mode, flow velocity: 1.5mL/min;
Sample size: 1.5 μ L;
The mass spectrophotometry condition:
Pattern: EI ionization pattern, ionization energy 70eV;
Ion source temperature: 230 ℃;
Quadrupole rod temperature: 150 ℃;
Transmission line temperature: 280 ℃;
Solvent delay 6min;
Scan mode: select ion monitoring (SIM) pattern;
At first each mixed standard solution is detected under above-mentioned gas chromatography and mass spectrum condition, the peak area of the organophosphorus pesticide that obtains and the ratio of internal standard compound peak area are carried out regretional analysis with the concentration of corresponding organophosphorus pesticide, calculate standard working curve and the regression equation thereof of each organophosphorus pesticide;
Secondly sample solution is detected under above-mentioned the same terms, the peak area of the organophosphorus pesticide that obtains and the ratio of internal standard compound peak area are brought in the corresponding regression equation, obtain the concentration of each organophosphorus pesticide in the sample solution, calculate the residual quantity of each organophosphorus pesticide in the sample.
The method of organophosphorus pesticide residual quantity in the detection tobacco of the present invention, adopting the mixed liquor with acetonitrile and acetone is the pre-treatment step of extractant, treatment step is simple, can effectively the object in the sample be extracted in the organic phase; And in the gaschromatographic mass spectrometric analysis process, acetone be fit to use more than acetonitrile, can improve the precision of detection, has therefore only added acetone soln at last in sample pre-treatments.
In addition, detection method of the present invention adopts PSA adsorbent and anhydrous magnesium sulfate that extract is purified, and is simple to operate, with low cost, and purification effects is good; In addition, the present invention is optimized the condition of gaschromatographic mass spectrometry, and it is highly sensitive to have proposed a mensuration, the detection method that accuracy is good, can detect the nearly residual quantity of 20 kinds of organophosphorus pesticides simultaneously, meet the development trend that in tobacco, detects organophosphorus pesticide residual quantity at present.
Description of drawings
Fig. 1 is mixed standard solution (1 μ g/g) GC-MS-SIM spectrogram; 1. DDVP among the figure, 2. Menite (two isomeride), 3. orthene, 4. thionazin, 5. terbufos, 6. disulfoton, 7. iprobenfos, 8. phosphamidon (two isomeride), 9. chlorpyrifos-methyl, 10. Nankor, 11. tolelofos-methyls, 12. parathion-methyls, 13. formothion, 14. fenifrothions, 15. ethyl parathions, 16. ethyl-pyrimidine phosphorus, 17. bromophos, 18. Rilariols, 19. chlorine third phosphorus, 20. azinphos-methyls, IS. isazofos.
Embodiment
One, below in conjunction with embodiment detection method of the present invention is done detailed explanation.
Detection method of the present invention relates to 20 kinds of organophosphorus pesticides: DDVP, Menite, orthene, thionazin, terbufos, disulfoton, iprobenfos, phosphamidon, chlorpyrifos-methyl, Nankor, tolelofos-methyl, parathion-methyl, formothion, fenifrothion, ethyl parathion, ethyl-pyrimidine phosphorus, bromophos, Rilariol, chlorine third phosphorus, azinphos-methyl.Detection method of the present invention is internal standard compound with the isazofos, specifically comprises the steps:
1) preparation of mixed standard solution:
Accurately take by weighing 20 kinds of organophosphorus pesticide standard items of 0.1g respectively in same 100ml volumetric flask, obtain hybrid standard storing solution A with the acetone constant volume, accurately pipette hybrid standard storing solution A 1ml in the 100ml volumetric flask, use the acetone constant volume, obtain hybrid standard storing solution B.Accurately pipette the hybrid standard storing solution B of 0.1ml, 0.5mL, 1mL, 2.5mL, 5mL respectively in the 100ml volumetric flask, add internal standard compound more respectively, use the acetone constant volume then, obtain the mixed standard solution of a series of variable concentrations, wherein the concentration of 20 kinds of organophosphorus pesticide standard items is respectively: 0.01 μ g/mL, 0.05 μ g/mL, 0.1 μ g/mL, 0.25 μ g/mL, 0.5 μ g/mL, interior mark concentration 0.5 μ g/mL.
2) pre-treatment of sample:
Accurately take by weighing and pulverize back, dried tobacco sample 1g, place the centrifuge tube of 50mL, add the 10mL ultrapure water and soak into 20min, add the 10mL acetonitrile then, jolting 1min adds 4g anhydrous magnesium sulfate, 1g sodium chloride and 5ml acetone, immediately jolting 2min again, prevent the anhydrous magnesium sulfate caking, in the centrifugal 10min of 7000 rpm.The upper strata acetonitrile layer 5mL that gets after centrifugal joins in the centrifuge tube that is placed with 150mg PSA adsorbent and 450mg anhydrous magnesium sulfate, and jolting 30s is in the centrifugal 10min of 10000 rpm.Draw supernatant liquor 4mL in the nitrogen bottle blowing, blow down at 40 ℃ of water-bath nitrogen and be concentrated into 0.1mL, be settled to 1mL with acetone again, through 0.22 μ m organic phase membrane filtration, obtain sample solution.
3) gaschromatographic mass spectrometric analysis:
Analytical conditions for gas chromatography:
Chromatographic column: DB-17MS elastic quartz capillary tube chromatographic column (30m * 0.32mm * 0.25 μ m);
Injector temperature: 270 ℃;
Temperature programme: 70 ℃ of initial temperatures keep 1min after keeping behind the 1min being raised to 150 ℃ with 15 ℃/min; Be raised to 190 ℃ with 1 ℃/min then, be raised to 270 ℃ with 15 ℃/min at last, keep 10min;
Input mode: split sampling not;
Carrier gas: helium, constant current mode, flow velocity: 1.5mL/min;
Sample size: 1.5 μ L.
The mass spectrophotometry condition:
Pattern: EI ionization pattern, ionization energy 70eV;
Ion source temperature: 230 ℃;
Quadrupole rod temperature: 150 ℃;
Transmission line temperature: 280 ℃;
Solvent delay 6min;
Scan mode: select ion monitoring (SIM) pattern.
The testing result of table 1 mixed standard solution
Two, following accuracy to detection method of the present invention is investigated:
Three mark-on levels are respectively 0.1 μ g/g, 0.5 μ g/g and 1 μ g/g, and the concentration of interior mark isazofos is 1 μ g/g, and each mark-on level repeats five times, according to measured quantity with add the recovery and the precision that scalar calculates each interpolation level.Concrete outcome sees Table 2.
The investigation result of table 2 detection method
The recovery of three mark-on levels of 20 kinds of organophosphorus pesticides is positioned between 70% ~ 118%, and relative standard deviation is 0.5% ~ 11.9%, illustrates that the measurement result of this method is comparatively reliable.
Three, adopt detection method of the present invention that concrete tobacco sample is detected:
Because the actual conditions difference that proportion of crop planting process agricultural chemicals uses, use pesticide variety that very big limitation is also arranged, analytic sample in residues of pesticides generally can not contain whole analytic targets, all adopts blank sample to add the target mode so verify the example of pesticide residue analysis method usually.Below adopt detection method of the present invention that three blind samples of blank mark-on are detected, add scalar and testing result is as shown in table 3.
The blind sample of the blank mark-on of table 3 add scalar and testing result
Claims (3)
1. method that detects organophosphorus pesticide residual quantity in the tobacco, it is characterized in that: comprise following sample pre-treatments: add tobacco sample weight 5-15 water logging bubble doubly, the extractant that adds every gram tobacco sample 10-20ml again extracts, carrying out centrifuging and taking part upper organic phase clear liquid after the extraction brushes concentrated through purified treatment, nitrogen, add acetone soln then, obtain sample solution through 0.22 μ m organic phase membrane filtration; Wherein extractant is the mixed liquor of acetonitrile and acetone, and the volume ratio of acetonitrile and acetone is 1-2:1; After the pre-treatment, be that internal standard compound adopts the organophosphorus pesticide residual quantity in the gaschromatographic mass spectrometry method test sample solution with the isazofos with the sample solution that obtains; Described organophosphorus pesticide is: DDVP, Menite, orthene, thionazin, terbufos, disulfoton, iprobenfos, phosphamidon, chlorpyrifos-methyl, Nankor, tolelofos-methyl, parathion-methyl, formothion, fenifrothion, ethyl parathion, ethyl-pyrimidine phosphorus, bromophos, Rilariol, chlorine third phosphorus, azinphos-methyl; Specifically comprise the steps:
1) preparation of mixed standard solution: get the mixed standard solution that each organophosphorus pesticide standard items is blended at least three concentration of preparation in the 0.01-1 μ g/ml concentration range, add the internal standard compound isazofos during preparation, the concentration of isazofos in each mixed standard solution is 0.5 μ g/ml;
2) pre-treatment of sample: accurately take by weighing the dry sample after the pulverizing, place centrifuge tube, add example weight 5-15 ultrapure water doubly and soak 20min, add acetonitrile, anhydrous magnesium sulfate, sodium chloride and acetone then, jolting 2min immediately is in the centrifugal 10min of 7000 rpm; Getting above-mentioned upper organic phase clear liquid after centrifugal joins in the centrifuge tube that is placed with PSA adsorbent and anhydrous magnesium sulfate, jolting 30s, in the centrifugal 10min of 10000 rpm, draw supernatant liquor in the nitrogen bottle blowing, blow down concentrated at 40 ℃ of water-bath nitrogen, add acetone soln again, through 0.22 μ m organic phase membrane filtration;
3) gaschromatographic mass spectrometric analysis:
Analytical conditions for gas chromatography:
Chromatographic column: DB-17MS elastic quartz capillary tube chromatographic column (30m * 0.32mm * 0.25 μ m);
Injector temperature: 270 ℃;
Temperature programme: 70 ℃ of initial temperatures keep 1min after keeping behind the 1min being raised to 150 ℃ with 15 ℃/min; Be raised to 190 ℃ with 1 ℃/min then, be raised to 270 ℃ with 15 ℃/min at last, keep 10min;
Input mode: split sampling not;
Carrier gas: helium, constant current mode, flow velocity: 1.5mL/min;
Sample size: 1.5 μ L;
The mass spectrophotometry condition:
Pattern: EI ionization pattern, ionization energy 70eV;
Ion source temperature: 230 ℃;
Quadrupole rod temperature: 150 ℃;
Transmission line temperature: 280 ℃;
Solvent delay 6min;
Scan mode: select ion monitoring (SIM) pattern;
At first each mixed standard solution is detected under above-mentioned gas chromatography and mass spectrum condition, the peak area of the organophosphorus pesticide that obtains and the ratio of internal standard compound peak area are carried out regretional analysis with the concentration of corresponding organophosphorus pesticide, calculate standard working curve and the regression equation thereof of each organophosphorus pesticide;
Secondly sample solution is detected under above-mentioned the same terms, the peak area of the organophosphorus pesticide that obtains and the ratio of internal standard compound peak area are brought in the corresponding regression equation, obtain the concentration of each organophosphorus pesticide in the sample solution, calculate the residual quantity of each organophosphorus pesticide in the sample.
2. according to the method for organophosphorus pesticide residual quantity in the described detection of claim 1 tobacco, it is characterized in that: also add anhydrous magnesium sulfate and the sodium chloride that saturating capacity is arranged during described extraction.
3. according to the described method that detects organophosphorus pesticide residual quantity in the tobacco of claim 1, it is characterized in that: described purified treatment is: the upper organic phase clear liquid after centrifugal is inserted in the container with PSA adsorbent and anhydrous magnesium sulfate, centrifugal treating is carried out in shaking again.
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| US8426212B2 (en) * | 2010-10-06 | 2013-04-23 | The Boeing Company | Method and system for monitoring for the presence of phosphate esters in jet fuel |
| CN102353567B (en) * | 2011-06-30 | 2013-08-21 | 河北工业大学 | Method for abstracting and enriching organic phosphorus in substrate sludge |
| CN102517230B (en) * | 2011-12-12 | 2013-06-19 | 温州医学院 | Bifidobacterium breve and detection method of methamidopho pesticide residue in foodstuff |
| CN102721762B (en) * | 2012-06-29 | 2014-04-16 | 晨光生物科技集团股份有限公司 | Method for detecting organophosphorus pesticide residues in capsanthin |
| CN103712846A (en) * | 2012-10-09 | 2014-04-09 | 吉林大学 | Method for treating organophosphorus pesticide residues in cereal beverage before detection |
| CN102866215B (en) * | 2012-10-17 | 2013-11-20 | 国家烟草质量监督检验中心 | Gas chromatography-mass spectrometer (GC-MS)/MS measuring method for 20 pesticide residues in tobaccos and tobacco products |
| CN103217496A (en) * | 2013-03-28 | 2013-07-24 | 国家烟草质量监督检验中心 | Method for measuring contents of humectants in cigarette cut tobacco by GC/FID (Gas Chromatography/hydrogen Flame Ionization Detector) |
| CN103293266B (en) * | 2013-06-08 | 2014-09-10 | 国家烟草质量监督检验中心 | GC-MS/MS (gas chromatography-tandem mass spectrometry) method for analyzing dinitroaniline pesticide residue in tobacco and tobacco product |
| CN103399099B (en) * | 2013-08-14 | 2014-08-06 | 山东农业大学 | Method for detecting nine organophosphorus pesticides simultaneously |
| CN104316640A (en) * | 2014-11-14 | 2015-01-28 | 山东省农业科学院农业质量标准与检测技术研究所 | Method for measuring organophosphorus pesticide residues in vegetables and fruits |
| CN109668990A (en) * | 2019-03-05 | 2019-04-23 | 河北大学 | The rapid assay methods of organophosphorus pesticide residue in a kind of vegetables |
| CN110441453B (en) * | 2019-08-14 | 2022-03-15 | 国家烟草质量监督检验中心 | Method for separating and detecting phosphamidon isomers |
| CN113740452B (en) * | 2021-08-04 | 2023-05-02 | 浙江药科职业大学 | Method for determining residual pesticide based on separation before room-temperature ionic liquid column |
| CN114252529A (en) * | 2021-12-24 | 2022-03-29 | 江苏赫尔斯检测技术有限公司 | Method for determining methyl parathion by tandem mass spectrometry |
| CN114354323B (en) * | 2022-01-17 | 2023-06-30 | 山西农业大学 | Method for determining parathion in grains by combining liquid-liquid microextraction of dispersion liquid based on hydrophilic and hydrophobic eutectic solvents and digital image colorimetric method |
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