CN104133023A - Analysis method for simultaneously detecting tralomethrin and deltamethrin in tobaccos by using bonded phase chromatography - Google Patents
Analysis method for simultaneously detecting tralomethrin and deltamethrin in tobaccos by using bonded phase chromatography Download PDFInfo
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Abstract
The invention provides an analysis method for simultaneously detecting tralomethrin and deltamethrin in tobaccos by using a bonded phase chromatography. The method is characterized by comprising the following steps: firstly, extracting residual tralomethrin and deltamethrin in tobacco base materials by using acetonitrile; adding a certain amount of magnesium sulfate, sodium chloride, dehydrated sodium citrate and sodium hydrogen citrate substances and oscillating; after centrifuging, sucking a certain amount of supernatant and carrying out nitrogen blowing concentration; after a certain concentration is reached, carrying out solid-phase extraction on the supernatant to carry out purification treatment; redissolving by using an acetonitrile solvent after nitrogen blowing; filtering the solution by an organic phase filter membrane with the size of 0.22 micron; and carrying out concentration analysis on tralomethrin and deltamethrin by using the super-efficient bonded phase chromatography. According to the method, the method for simultaneously and rapidly detecting tralomethrin and deltamethrin in the tobaccos is established for the first time by utilizing a UPC2. According to the technology, CO2 is taken as a main mobile phase and separation and quantitative analysis on two compounds can be realized within eight minutes, so that evidences are provided for a related test of an index.
Description
technical field:
The present invention relates to the Detection Technologies of Pesticide Residues field, specifically the quantitative analysis method of tralomethrin and deltamethrin residues in tobacco is closed phase chromatogram and is detected simultaneously in a kind of utilization.
background technology:
Tralomethrin be a kind of decis and bromine obtain by addition reaction there is highly active anti-insects agricultural chemicals, comprise altogether two isomeride.This agricultural chemicals has very significant effect for multiple insect in the tobaccos such as control coleoptera, Diptera, Semiptera, is therefore widely used in the plantation of tobacco.Decis itself is also a kind of pesticide, and lepidopterous larvae is had to good prevention effect, is often used to the protection of planting process to tobacco crop.Tralomethrin and decis not only have harm to the hydrobiont such as fish, shrimp and useful insect, the residual health hazard risk that also can increase the weight of smoker and surrounding population in tobacco.Therefore, to these two kinds of agricultures that exist in tobacco residual monitor significant.
Tralomethrin and decis structurally have very large similarity, detect and have higher difficulty simultaneously.At present, the detection method of the tralomethrin of report is mainly vapor-phase chromatography (GC), gas chromatography-mass spectrography (GC-MS) and high performance liquid chromatography (HPLC) both at home and abroad.Wherein, being most widely used of gas chromatography.But, under high temperature action due to the 280 DEG C of left and right of injection port in gas chromatography, there is to decompose generation decis in tralomethrin, what utilize that in fact vapor-phase chromatography record can only be the total amount that tralomethrin transforms decis and existing decis itself, can not distinguish quantitatively these two kinds of residues of pesticides.And close phase chromatographic run temperature general control 50 DEG C of left and right, at this temperature, tralomethrin stable in properties, do not find to change into the phenomenon of decis, therefore, utilization is closed tralomethrin and the decis that phase chromatogram detects in tobacco simultaneously and is had certain actual application value, can understand better tobacco Pesticide Residues situation.
summary of the invention:
The analytical approach of tralomethrin and decis in tobacco is closed phase chromatogram and is detected simultaneously in a kind of utilization that object of the present invention provides based on above-mentioned prior art situation just, with emerging express-analysis when closing phase chromatographic technique and complete in tobacco tralomethrin and decis, mainly first to utilize QuRChERS pretreatment technology and solid phase extraction techniques to carry out pre-service, then adopt ultra high efficiency to close chromatography tralomethrin and decis are detected simultaneously, and carry out quantitative test by external standard method.This method instrumental analysis is quick, and consumption of organic solvent is few, is a kind of analytical approach that integrates the multiple advantage such as efficient, sensitive, green.
The object of the invention is to be achieved through the following technical solutions:
The analytical approach of tralomethrin and decis in tobacco is closed phase chromatogram and is detected simultaneously in a kind of utilization, first utilize acetonitrile to extract tralomethrin residual in tobacco matrix and decis, add a certain amount of magnesium sulfate, sodium chloride, Sodium citrate dehydrate, natrium hydrocitricum vibrates, a certain amount of supernatant of centrifugal rear absorption carries out nitrogen and blows concentrated, reach after finite concentration, carry out Solid-Phase Extraction it is carried out to purified treatment, after drying up, nitrogen utilize acetonitrile solvent to redissolve, cross after 0.22 μ m organic phase filter membrane, utilize ultra high efficiency to close chromatography tralomethrin and decis are wherein carried out to concentration analysis, concrete steps are as follows:
1) extraction of sample
For obtaining good extraction effect, first take tobacco sample that 2.0 g have pulverized in 50 mL tool plug centrifuge tubes, add 10 mL ultrapure waters to infiltrate sample, leave standstill 10 min, get 10 mL acetonitriles in centrifuge tube, on vortex mixer, with 2000 rpm velocity fluctuation 1 min, centrifuge tube is put into-20 ° of C refrigerator freezing 10 min, to prevent that the heat production in salting-out process from causing some target substance to decompose.Then in centrifuge tube, add the pack of saltouing (containing 4 g anhydrous magnesium sulfates, 1 g sodium chloride, 1 g sodium citrate and 0.5 g DisodiumHydrogen Citrate), immediately on vortex mixer with 2000 rpm, 2 min that vibrate, with centrifugal 3 min of 5000 rpm, get 5mL supernatant liquid nitrogen and blow and be concentrated into 1mL;
2) Solid phase extraction of sample
Adopt florisil silica pillar as solid-phase extraction column, the mixed liquor (95:5, v/v) of normal hexane and acetone, as eluent, carries out Solid phase extraction processing to the sample having concentrated, concrete operation step is divided into: first, utilize 6 mL eluents to carry out activation processing to florisil silica pillar; Secondly, the 1mL concentrate that previous step is obtained is injected on florisil silica pillar; The 3rd step, utilizes 5 ml eluents to wash pillar, collects whole cleansing solutions; The 4th step, injects 3 mL air with liquid residual on emptying pillar; This step can reduce the matrix interference in tobacco sample effectively.
3) concentrate, redissolve and filter
Close carrying out smoothly of chromatography analytical work for ensureing ultra high efficiency, realize accurate quantification simultaneously, need be 1 mL acetonitrile by extract solvent replacement, concrete way is: first concentrated near dry to the eluent of collecting with Nitrogen evaporator, then add 1 mL acetonitrile to redissolve, and utilize 0.22 μ m organic phase filter membrane to filter sample, as sample liquid to be measured;
4) standard operation solution preparation
The concrete grammar of standard operation solution preparation is as follows:
Tralomethrin and decis list mark storing solution: accurately take 10.0 mg(and be accurate to 0.1 mg) standard items, be placed in 10 mL volumetric flasks, dissolve constant volume with acetonitrile, being mixed with mass concentration is single mark storing solution of 1000.0 μ g/mL, is stored in-20 ° of C refrigerators for subsequent use;
Hybrid standard working solution: get respectively tralomethrin and decis list mark storing solution 0.5ml in 100 mL volumetric flasks, use dilution in acetonitrile constant volume, be mixed with the hybrid working storing solution that two kinds of pesticide composition mass concentrations are respectively 5.0 μ g/mL, be stored in 4 ° of C refrigerators for subsequent use;
Series standard solution preparation: the hybrid standard working solution that accurately pipettes 0.2 mL, 0.5 mL, 1 mL, 2 mL, 5 mL, be placed in 10 mL volumetric flasks, use acetonitrile constant volume, obtain series standard working solution, concrete concentration is: 0.1 μ g/mL, 0.25 μ g/mL, 0.5 μ g/mL, 1.0 μ g/mL, 2.5 μ g/mL, 5.0 μ g/mL.
5) close analysis of hplc
Adopt ultra high efficiency to close chromatography standard operation solution and sample liquid to be measured are carried out to concentration analysis, UV-detector detects, and external standard method is quantitative;
Chromatographic condition: adopting chromatographic column is Acquity UPC
2cSH Fluoro-Phenyl chromatographic column; ABPR pressure is 1800 psi; Chromatogram column temperature is 40 DEG C; Sample size is 5-10 μ L; Mobile phase is respectively CO
2(mobile phase A) and methyl alcohol (Mobile phase B), flow velocity is 1.5 mL/min, eluent gradient elution program is as table 1; It is 215 nm that ultraviolet detects wavelength;
Table 1 gradient elution program
6) method evaluation
Close under phase chromatographic condition above-mentioned, this method is evaluated, the linear equation of tralomethrin and decis composition, the range of linearity, related coefficient, average recovery rate, quantitative limit etc. are in table 2:
This method is utilized UPC first
2set up a kind of Rapid Simultaneous Determination method that simultaneously detects tralomethrin and decis in tobacco.With supercritical CO
2be main,, improved the efficiency of stratographic analysis, and reduced largely organic solvent use amount as mobile phase in conjunction with a small amount of acetonitrile, reduced the pollution to environment, alleviate the health threat of analytic process to operating personnel.Can in 8 minutes, realize the Simultaneous Quantitative Analysis of tralomethrin and decis, the vapor-phase chromatography of having filled up current normal employing can not be distinguished the deficiency of these two kinds of objects of quantitative test simultaneously.This method can provide foundation for the related check of above-mentioned two kinds of objects.
brief description of the drawings:
Fig. 1: sample pre-treatments and close phase chromatogram overhaul flow chart.
Fig. 2: close phase chromatogram.Wherein, 1 is decis; 2,3 is two kinds of isomeride of tralomethrin (while showing sample introduction for giving prominence to, conversion reaction generation decis does not occur tralomethrin, two class target compounds is not placed on same chromatogram).
embodiment:
The present invention is described further in conjunction with example, but is not restriction the present invention.
Example 1:
1. instrument and reagent:
Tralomethrin and decis: be standard items; Acetonitrile, acetone, normal hexane, be chromatographic grade reagent.
U.S. Waters closes chromatography (UPC
2), Switzerland Mettler AE 163 electronic balances (sensibility reciprocal: 0.0001g); U.S. Labnet VtexMixer VX200 oscillator; Germany Sigma high speed freezing centrifuge.
2. sample preparation:
Certain burley tobaccos sample is analyzed, first carried out the extraction of sample: take respectively tobacco sample that 2.0 g have pulverized in 50 mL tool plug centrifuge tubes, add 10 mL water infiltration samples, leave standstill 10 min.Get 10 mL acetonitriles in centrifuge tube, on vortex mixer, with 2000 rpm velocity fluctuation 1 min, centrifuge tube is put into-20 DEG C of refrigerator freezing 10 min.Then to adding the pack of saltouing (containing 4 g anhydrous magnesium sulfates, 1 g sodium chloride, 1 g sodium citrate and 0.5 g DisodiumHydrogen Citrate) in centrifuge tube, immediately on vortex mixer with 2000 rpm, 2 min that vibrate, with centrifugal 3 min of 5000 rpm.Getting 5 mL supernatant liquid nitrogen blows and is concentrated into 1 mL.
Secondly, the sample having concentrated is carried out to Solid phase extraction processing, concrete operation step is divided into: first, utilize the mixed liquor (95:5) of 6 mL normal hexanes and ethyl acetate to carry out activation processing to florisil silica pillar; Secondly, the 1 mL concentrate that previous step is obtained is injected on florisil silica pillar; The 3rd step, utilizes normal hexane that 5 ml volume ratios are 95:5 and the mixed liquor of acetone to wash pillar, collects whole cleansing solutions; The 4th step, injects 3 mL air with liquid residual on emptying pillar.Treating fluid is concentrated, redissolved and 0.22 μ m organic phase filter membrane filters sample.
3. standard solvent configuration:
The tralomethrin of preparation and the series standard solution concentration of decis are: 0.1 μ g/mL, 0.25 μ g/mL, 0.5 μ g/mL, 1.0 μ g/mL, 2.5 μ g/mL, 5.0 μ g/mL.
4. measure:
Employing is closed phase chromatogram and respectively standard operation solution and sample liquid to be measured is analyzed, and UV-detector detects, and external standard method is quantitative.
Chromatographic condition: adopting chromatographic column is Acquity UPC
2cSH Fluoro-Phenyl chromatographic column; ABPR pressure is 1800 psi; Chromatogram column temperature is 60 DEG C; Sample size is 5-10 μ L; Mobile phase is respectively CO
2(mobile phase A) and methyl alcohol (Mobile phase B), flow velocity is 1.5 mL/min, eluent gradient elution program is as table 1; It is 215 nm that ultraviolet detects wavelength.Analysis result is in table 3.
Analysis result:
table 3 actual sample testing result (unit: mg/kg)
| Decis | Tralomethrin |
| 0.56 | 0.43 |
Example 2:
As described in Example 1, select another tobacco sample B(flue-cured tobacco sample), record the content of 2 kinds of agricultural chemicals objects in sample in table 4.
table 4 actual sample testing result (unit: mg/kg)
| Decis | Tralomethrin |
| 0.61 | — |
Note: "-" representative does not detect
Example 3: select sample C(finished cigarettes), cigarette is only split and collects pipe tobacco, to pulverize, other operate as described in Example 1, record the content of 2 class agricultural chemicals objects in sample in table 5.
table 5 actual sample testing result (unit: mg/kg)
| Decis | Tralomethrin |
| — | — |
Note: "-" representative does not detect
Claims (3)
1. the analytical approach of tralomethrin and decis in tobacco is closed phase chromatogram and is detected simultaneously in a utilization, it is characterized in that: first utilize acetonitrile to extract tralomethrin residual in tobacco matrix and decis, add a certain amount of magnesium sulfate, sodium chloride, Sodium citrate dehydrate, natrium hydrocitricum vibrates, a certain amount of supernatant of centrifugal rear absorption carries out nitrogen and blows concentrated, reach after finite concentration, carry out Solid-Phase Extraction it is carried out to purified treatment, after drying up, nitrogen utilize acetonitrile solvent to redissolve, cross after 0.22 μ m organic phase filter membrane, utilize ultra high efficiency to close chromatography tralomethrin and decis are wherein carried out to concentration analysis.
2. the analytical approach of tralomethrin and decis in tobacco is closed phase chromatogram and is detected simultaneously in utilization according to claim 1, it is characterized in that: the concrete steps of described analytical approach are as follows:
1) extraction of sample
First take tobacco sample that 2.0 g have pulverized in 50 mL tool plug centrifuge tubes, add 10 mL ultrapure waters to infiltrate sample, leave standstill 10 min, get 10 mL acetonitriles in centrifuge tube, on vortex mixer with 2000 rpm velocity fluctuation 1 min, centrifuge tube is put into-20 ° of C refrigerator freezing 10 min, then in centrifuge tube, add the pack of saltouing (containing 4 g anhydrous magnesium sulfates, 1 g sodium chloride, 1 g sodium citrate and 0.5 g natrium hydrocitricum), immediately on vortex mixer with 2000 rpm, 2 min that vibrate, with centrifugal 3 min of 5000 rpm, getting 5mL supernatant liquid nitrogen blows and is concentrated into 1mL,
2) Solid phase extraction of sample
Adopt florisil silica pillar as solid-phase extraction column, the mixed liquor (95:5, v/v) of normal hexane and acetone, as eluent, carries out Solid phase extraction processing to the sample having concentrated, concrete operation step is divided into: first, utilize 6 mL eluents to carry out activation processing to florisil silica pillar; Secondly, the 1mL concentrate that previous step is obtained is injected on florisil silica pillar; The 3rd step, utilizes 5 ml eluents to wash pillar, collects whole cleansing solutions; The 4th step, injects 3 mL air with liquid residual on emptying pillar;
3) concentrate, redissolve and filter
First concentrated near dry to the eluent of collecting with Nitrogen evaporator, then add 1 mL acetonitrile to redissolve, and utilize 0.22 μ m organic phase filter membrane to filter sample, as sample liquid to be measured;
4) standard operation solution preparation
The series standard solution concentration of tralomethrin and decis is: 0.1 μ g/mL, 0.25 μ g/mL, 0.5 μ g/mL, 1.0 μ g/mL, 2.5 μ g/mL, 5.0 μ g/mL;
5) close analysis of hplc
Adopt ultra high efficiency to close chromatography standard operation solution and sample liquid to be measured are carried out to concentration analysis, UV-detector detects, and external standard method is quantitative;
Chromatographic condition: adopting chromatographic column is Acquity UPC
2cSH Fluoro-Phenyl chromatographic column; ABPR pressure is 1800 psi; Chromatogram column temperature is 40 DEG C; Sample size is 5-10 μ L; Mobile phase is respectively CO
2(mobile phase A) and methyl alcohol (Mobile phase B), flow velocity is 1.5 mL/min, eluent gradient elution program is as table 1; It is 215 nm that ultraviolet detects wavelength;
Table 1 gradient elution program
。
3. the analytical approach of tralomethrin and decis in tobacco is closed phase chromatogram and is detected simultaneously in utilization according to claim 1, it is characterized in that: the concrete grammar of standard operation solution preparation is as follows:
Tralomethrin and decis list mark storing solution: accurately take 10.0 mg(and be accurate to 0.1 mg) standard items, be placed in 10 mL volumetric flasks, dissolve constant volume with acetonitrile, being mixed with mass concentration is single mark storing solution of 1000.0 μ g/mL, is stored in-20 ° of C refrigerators for subsequent use;
Hybrid standard working solution: get respectively tralomethrin and decis list mark storing solution 0.5ml in 100 mL volumetric flasks, use dilution in acetonitrile constant volume, be mixed with the hybrid working storing solution that two kinds of pesticide composition mass concentrations are respectively 5.0 μ g/mL, be stored in 4 ° of C refrigerators for subsequent use;
Series standard solution preparation: the hybrid standard working solution that accurately pipettes 0.2 mL, 0.5 mL, 1 mL, 2 mL, 5 mL, be placed in 10 mL volumetric flasks, use acetonitrile constant volume, obtain series standard working solution, concrete concentration is: 0.1 μ g/mL, 0.25 μ g/mL, 0.5 μ g/mL, 1.0 μ g/mL, 2.5 μ g/mL, 5.0 μ g/mL.
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| CN106814155A (en) * | 2017-03-10 | 2017-06-09 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine close phase chromatographic tandem mass spectrography in a kind of tomato |
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| CN106770745A (en) * | 2016-12-08 | 2017-05-31 | 南京财经大学 | The method of decis in detection powdered rice hulls or coarse rice powder |
| CN106814155A (en) * | 2017-03-10 | 2017-06-09 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine close phase chromatographic tandem mass spectrography in a kind of tomato |
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| CN106896173A (en) * | 2017-03-10 | 2017-06-27 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine close phase chromatographic tandem mass spectrography in a kind of electronic cigarette liquid |
| CN106896174A (en) * | 2017-03-10 | 2017-06-27 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine close phase chromatographic tandem mass spectrography in a kind of smoke-free tobacco product |
| CN106896175A (en) * | 2017-03-10 | 2017-06-27 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine close phase chromatographic tandem mass spectrography in a kind of Ling " for giving up smoking |
| CN106841454B (en) * | 2017-03-10 | 2019-05-10 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of bolete |
| CN106814155B (en) * | 2017-03-10 | 2019-05-17 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of tomato |
| CN114636763A (en) * | 2022-01-27 | 2022-06-17 | 贵州健安德科技有限公司 | Method for simultaneously detecting dinotefuran and deltamethrin pesticide residues in crops |
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