CN105866320A - Organophosphorus pesticide dimethoate residue detection method based on silica gel plate chromatography - Google Patents
Organophosphorus pesticide dimethoate residue detection method based on silica gel plate chromatography Download PDFInfo
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- CN105866320A CN105866320A CN201610386110.5A CN201610386110A CN105866320A CN 105866320 A CN105866320 A CN 105866320A CN 201610386110 A CN201610386110 A CN 201610386110A CN 105866320 A CN105866320 A CN 105866320A
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- Prior art keywords
- silica gel
- liquid
- gel plate
- calcein
- solution
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- MCWXGJITAZMZEV-UHFFFAOYSA-N dimethoate Chemical group CNC(=O)CSP(=S)(OC)OC MCWXGJITAZMZEV-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 238000001514 detection method Methods 0.000 title claims abstract description 53
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000000741 silica gel Substances 0.000 title claims abstract description 31
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 31
- 238000004587 chromatography analysis Methods 0.000 title claims abstract description 28
- 239000003987 organophosphate pesticide Substances 0.000 title claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 55
- DEGAKNSWVGKMLS-UHFFFAOYSA-N calcein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC(CN(CC(O)=O)CC(O)=O)=C(O)C=C1OC1=C2C=C(CN(CC(O)=O)CC(=O)O)C(O)=C1 DEGAKNSWVGKMLS-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229960002378 oftasceine Drugs 0.000 claims abstract description 48
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 239000000843 powder Substances 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 14
- 239000003905 agrochemical Substances 0.000 claims description 10
- 230000009514 concussion Effects 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- 229940079593 drug Drugs 0.000 claims description 4
- 239000003814 drug Substances 0.000 claims description 4
- 238000007689 inspection Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 24
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000005947 Dimethoate Substances 0.000 abstract 2
- 238000004519 manufacturing process Methods 0.000 abstract 2
- 230000005855 radiation Effects 0.000 abstract 2
- 238000001917 fluorescence detection Methods 0.000 abstract 1
- 238000005360 mashing Methods 0.000 abstract 1
- 238000004809 thin layer chromatography Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 57
- 238000006243 chemical reaction Methods 0.000 description 24
- 239000000463 material Substances 0.000 description 23
- 239000000126 substance Substances 0.000 description 17
- 238000012360 testing method Methods 0.000 description 13
- 239000007864 aqueous solution Substances 0.000 description 11
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 8
- GRWQEXZZWRVXDZ-UHFFFAOYSA-N 2,6,7-trihydroxy-9-(2-hydroxyphenyl)xanthen-3-one Chemical class C1=2C=C(O)C(O)=CC=2OC2=CC(=O)C(O)=CC2=C1C1=CC=CC=C1O GRWQEXZZWRVXDZ-UHFFFAOYSA-N 0.000 description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 6
- 238000002795 fluorescence method Methods 0.000 description 6
- 239000000575 pesticide Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 229910001961 silver nitrate Inorganic materials 0.000 description 5
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 4
- 238000010790 dilution Methods 0.000 description 4
- 239000012895 dilution Substances 0.000 description 4
- 235000013399 edible fruits Nutrition 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 230000000536 complexating effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 229910000474 mercury oxide Inorganic materials 0.000 description 3
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 239000012286 potassium permanganate Substances 0.000 description 3
- 238000006479 redox reaction Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 235000013311 vegetables Nutrition 0.000 description 3
- LOTKRQAVGJMPNV-UHFFFAOYSA-N 1-fluoro-2,4-dinitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(F)C([N+]([O-])=O)=C1 LOTKRQAVGJMPNV-UHFFFAOYSA-N 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229910001447 ferric ion Inorganic materials 0.000 description 2
- GNBHRKFJIUUOQI-UHFFFAOYSA-N fluorescein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC=C(O)C=C1OC1=CC(O)=CC=C21 GNBHRKFJIUUOQI-UHFFFAOYSA-N 0.000 description 2
- 235000012055 fruits and vegetables Nutrition 0.000 description 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- 235000013336 milk Nutrition 0.000 description 2
- 239000002574 poison Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- XIAYFENBYCWHGY-UHFFFAOYSA-N 2-[2,7-bis[[bis(carboxymethyl)amino]methyl]-3-hydroxy-6-oxoxanthen-9-yl]benzoic acid Chemical compound C=12C=C(CN(CC(O)=O)CC(O)=O)C(=O)C=C2OC=2C=C(O)C(CN(CC(O)=O)CC(=O)O)=CC=2C=1C1=CC=CC=C1C(O)=O XIAYFENBYCWHGY-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 102000003914 Cholinesterases Human genes 0.000 description 1
- 108090000322 Cholinesterases Proteins 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- FHNINJWBTRXEBC-UHFFFAOYSA-N Sudan III Chemical compound OC1=CC=C2C=CC=CC2=C1N=NC(C=C1)=CC=C1N=NC1=CC=CC=C1 FHNINJWBTRXEBC-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000031709 bromination Effects 0.000 description 1
- 238000005893 bromination reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229940048961 cholinesterase Drugs 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229960001399 clenbuterol hydrochloride Drugs 0.000 description 1
- OPXKTCUYRHXSBK-UHFFFAOYSA-N clenbuterol hydrochloride Chemical compound Cl.CC(C)(C)NCC(O)C1=CC(Cl)=C(N)C(Cl)=C1 OPXKTCUYRHXSBK-UHFFFAOYSA-N 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- MHMNJMPURVTYEJ-UHFFFAOYSA-N fluorescein-5-isothiocyanate Chemical compound O1C(=O)C2=CC(N=C=S)=CC=C2C21C1=CC=C(O)C=C1OC1=CC(O)=CC=C21 MHMNJMPURVTYEJ-UHFFFAOYSA-N 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000002496 gastric effect Effects 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- -1 oxonium ion Chemical class 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000019633 pungent taste Nutrition 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000007447 staining method Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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- Health & Medical Sciences (AREA)
- Immunology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Optics & Photonics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Molecular Biology (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses an organophosphorus pesticide dimethoate residue detection method based on silica gel plate chromatography. The method comprises the following steps: preparing detection liquid, calcein and a CTMAB raw solution; mixing in a volume ratio of 1 to 2, so as to obtain detection liquid; carrying out thin layer chromatography on a silica gel plate by drowise adding to-be-tested target mashing liquid at one end of the silica gel plate; after complete chromatography, dropwise adding detection liquid prepared in the step S1 to the position farthest from a dropwise adding point; putting the silica gel plate into a darkroom, carrying out ultraviolet light radiation, and observing whether obvious yellow green fluorescence is produced, wherein the production of the fluorescence presents excessive residue. After being combined with dimethoate, the capability of CTMAB is stronger than calcein, and after the detection liquid is in contact with dimethoate, the ultraviolet light radiation is carried out in the darkroom, so that the production of the fluorescence can be obviously observed by naked eyes. By virtue of an indirect fluorescence detection principle, the judgment can be finished by observing through the naked eyes, and the detection of dimethoate residue is rapidly and conveniently realized.
Description
Technical field
The present invention relates to a kind of organophosphorus pesticide Determination of Dimethoate Residues detection method based on silica gel plate chromatography.
Background technology
Since new century, China experiencings earth-shaking change, economical, military, science and technology, cultural and educational level all to
World powers to stride forward, but the food-safety problem emerged in an endless stream in recent years is worth people's deep thinking.The tonyred event of 2006,08
Year Sanlu milk powder case, " leather milk ", the clenbuterol hydrochloride of 11 years, plastifying liquid, " the corpse meat " of 15 years and the ground always existed
Ditch oil, these are the most also tip of the iceberg, and food-safety problem is extremely urgent.On the other hand, for the vegetable and fruit of safety, I
Be still to worry its pesticide variety whether specification, whether amount exceeds standard, it may be said that this is the region that management difficulty is bigger comparatively speaking.
And Rogor to be one begin to use time is early, the common pesticides that range is wide, its sterling is white, needle-shaped crystals；It is slightly soluble in
Water, is soluble in alcohol；Ratio water weight, presents milky after being dissolved in water；There is pungent taste；Stable in acid condition, alkalescence bar
Easily decomposing under part, chance naked light high temperature is flammable, discharges the hypertoxic oxide of phosphorus, sulphur；Easily it is absorbed by plants and conducts to whole strain and plant
Thing, has the effect of Insecticiding-miticiding.After the Rogor of human contact's excess, internal cholinesterase activity can be suppressed, cause physiology merit
Can be disorderly.
Laboratory the most accurate can must record the content of residues of pesticides, kind, can allow and put a set of very large inspection in Common People
Survey instrument also the most unrealistic, be badly in need of on the market one quickly, Determination of Dimethoate Residues detection means easily.
Owing to the amount radix of residues of pesticides is smaller, and some agricultural chemicals is easily absorbed by plants so that vegetable surface is residual
The pesticide volume deposited is fewer, and can not represent the total amount of agricultural chemicals, therefore devises a kind of chromatography to be enriched with in plant residual
Agricultural chemicals.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of organophosphorus pesticide based on silica gel plate chromatography
Determination of Dimethoate Residues detection method, utilizes the not hydrophily (chromatography completely after can be farthest from instilling point) of Rogor, instills point in distance
Detecting liquid at a distance and without instilling at chromatography, utilize indirect fluorescent Cleaning Principle, observe the color distortion at two, naked eyes can be complete
Become to judge, quickly and conveniently realize the detection of Determination of Dimethoate Residues.
It is an object of the invention to be achieved through the following technical solutions: organophosphorus pesticide Rogor based on silica gel plate chromatography
Method for detecting residue, comprises the following steps:
S1: preparation detection liquid, including following sub-step:
S101: prepare original solution:
(1) take calcein powder, be dissolved in the first solvent, be configured to the concentration calcein not less than 0.05 mol/L molten
Liquid；Calcein (Calcein), molecular formula is C30H26N2O13, for fields such as complexometric indicator fluorescence indicators；Calcium is yellow
Green element is glassy yellow powder, is dissolved in ethanol and alkali, is slightly soluble in water, and its sodium salt is orange red crystallization, is dissolved in water, has green in yellow
Look fluorescence, insoluble in absolute ethyl alcohol and ether, fusing point is more than 300 DEG C.
(2) take cetyl trimethylammonium bromide powder, be dissolved in the second solvent, be configured to concentration and be not less than
The cetyl trimethylammonium bromide solution of 0.025mol/L；The molecular formula of CTMAB is C16H33 (CH3) 3NBr, white or
Light yellow crystals body, to powder, has penetrating odor, is soluble in isopropanol, water soluble, produces a large amount of foam during concussion, can be with
Cation, nonionic, amphoteric surfactant have good compatibility.There is excellent infiltration, softening, emulsification, antistatic, raw
The performances such as thing degradability and sterilization.Chemical stability is good, heat-resisting, fast light, pressure, strong alkali-acid resistance.Analytical chemistry is commonly used
A kind of surfactant, adding CTMAB in the mensuration of material can increase the degree of accuracy and the sensitivity of analysis.
S102: be the ratio of 1:2 according to volume ratio, the calcein solution that will have configured and cetyl trimethyl bromination
Ammonium salt solution mixes, and concussion obtains detecting liquid gently；
S2: colorimetric detection, including following sub-step:
S201: use tlc silica gel plate, smashs liquid to pieces in its one end instillation target to be measured and chromatographs；
S202: after chromatography is complete, instills some farthest in distance and instills the detection liquid obtained by step S1；
S203: be placed in darkroom by silica gel plate and irradiate with ultraviolet light, observes and drips whether there is obvious yellow-green fluorescence at detection liquid
Produce, if there being obvious yellow-green fluorescence to produce, having excessive organophosphorus pesticide Determination of Dimethoate Residues, otherwise then there is no excessive organophosphor
Agricultural chemicals Determination of Dimethoate Residues.
The concentration of described calcein solution is 1mol/L, and the concentration of described cetyl trimethylammonium bromide solution is
0.5mol/L。
Described calcein solution is 1:2 with the volume ratio of described cetyl trimethylammonium bromide solution.
The first described solvent is water.
The second described solvent is deionized water.
Organophosphorus pesticide Determination of Dimethoate Residues detection method based on silica gel plate chromatography, comprises the following steps:
S1: preparation detection liquid, including following sub-step:
S101: prepare original solution:
(1) take calcein powder, be dissolved in the first solvent, be configured to the concentration calcein not less than 0.05 mol/L molten
Liquid；
(2) take cetyl trimethylammonium bromide powder, be dissolved in the second solvent, be configured to concentration not less than 0.025mol/L's
Cetyl trimethylammonium bromide solution；
S102: be the ratio of 1:2 according to volume ratio, by molten with cetyl trimethylammonium bromide for the calcein solution configured
Liquid mixes, and concussion obtains detecting liquid gently；
S2: colorimetric detection, including following sub-step:
S201: use tlc silica gel plate, smashs liquid to pieces in its one end instillation target to be measured and chromatographs；
S202: after chromatography is complete, instills some farthest and without being respectively dropped into the inspection obtained by step S1 at chromatography in distance
Survey liquid；
S203: observe and whether have obvious color distortion at above-mentioned two, if there being obvious color distortion, has excessive organophosphor agriculture
Medicine Determination of Dimethoate Residues, on the contrary then there is no excessive organophosphorus pesticide Determination of Dimethoate Residues.
Cetyl trimethylammonium bromide CTMAB can react with calcein, can react with Rogor again, and it can be yellow with calcium
Green element complexing, reduces the fluorescence intensity of calcein, and makes fluorescence red shift, and CTMAB combines the ability of Rogor, and to be better than calcium yellowish green
Element, after detection liquid contact Rogor, irradiates with ultraviolet light in darkroom, and naked eyes can substantially observe that yellow-green fluorescence produces.
Drying method is that lucifuge natural air drying or high temperature are dried or low temperature drying.
The concentration of described calcein solution is 1mol/L, and the concentration of described cetyl trimethylammonium bromide solution is
0.5mol/L。
Described calcein solution is 1:2 with the volume ratio of described cetyl trimethylammonium bromide solution.
The first described solvent is water.
The second described solvent is deionized water.
The invention has the beneficial effects as follows:
1) cetyl trimethylammonium bromide CTMAB can react with calcein, can react with Rogor again, and it can be yellowish green with calcium
Element complexing, reduces the fluorescence intensity of calcein, and makes fluorescence red shift, and CTMAB combines the ability of Rogor and is better than calcein,
After detection liquid contact Rogor, irradiating with ultraviolet light in darkroom, naked eyes can substantially observe that yellow-green fluorescence produces.Utilize
Such indirect fluorescent Cleaning Principle, observes by the naked eye fluorescence and can complete to judge, quickly and conveniently achieve Determination of Dimethoate Residues
Detection.
2) fluorescence colour has the advantage that compared to other color reaction methods
One, colouring is more difficult finds a kind of suitably chemical substance.Chemical color method majority is that the character of inorganic compound is anti-
Should, mainly include decomposition reaction, combination reaction, metathesis reaction and displacement reaction.Want to go acquisition to deposit by color change
Possibility at a kind of material needs to look for a kind of color by above-mentioned fundamental reaction mode and changes substantially, reacts precision height
Material, this difficulty is the biggest, and organic reactive mode kind is more, and is more difficult to control its reaction process and reaction knot
Really, so, common color reaction is to be difficult to for the residual detecting a kind of material.
Its two, general chemistry reaction interference bigger.Chemical reaction is mainly with interionic reaction, group, sense
Reaction between group is main, which results in comparable ionic, group, the impact of functional group are the most fatal, such as silver ion
Reaction, if use is not deionized water, if the chloride ion content in water is higher, also easily produce muddy showing
As, so being difficult to accurately determine the material that strictly we are wanted being detected only by visually observing, and use
Fluorescence method is just with having arrived the physical property of material, and key reaction is absorption and complexing, and the interference of other materials is relatively low.
Its three, fluorescence method result is obvious.General color reaction more difficult direct judgement concentration is extremely low when, such as, three
The color change of valency iron, it becomes faint yellow from light yellow, examines and really can find to be varied from, if departing from reality
Testing the subjective idea of room, the when of removing to evaluate a kind of material color objectively, light yellow and faint yellow being difficult to is differentiated.And it is glimmering
Light method has natural advantage on observing, and has unstressed configuration to have only in darkroom and can judge with ultra violet lamp, and, i.e.
Make that compound concentration is relatively low makes fluorescence intensity relatively low, also can substantially comparison go out with and without difference.
Quite have superiority, either from side in view of all of the above, it is evident that fluorescence method seems as the effective ways detecting Determination of Dimethoate Residues
Formula, interference, result are analyzed up, will be better than general colouring, and fluorescence method can not only detect the existence of Rogor, moreover it is possible to
Utilize the instrument in laboratory, by the change of fluorescence intensity, accurately record the content of Rogor.
3) can be affected by factors such as decomposition, washings in view of the residual that Rogor is actual so that its ratio is less than 1:1000,
Use in laboratory the ratio of 1:1500,1:3000 to carry out test paper experiment, under this ratio, remain to tell Rogor be implicitly present in
Residual.But due to the Determination of Dimethoate Residues that country (GB 8,978 1996) allows is in water, two grades: 1.0mg/L tri-grade:
2.0mg/L, on fruits and vegetables, (GB 5,127 85) is 1.0mg/kg, if use 1:1000 Rogor spray solution, after 7 days its
Concentration just can reach fruits and vegetables national standard level, two grades of levels of waste water, so, accuracy of detection can reach actual requirement.
4) silica gel plate chromatography can effectively be enriched with in plant to be measured the agricultural chemicals of residual, solves persticide residue radix
Little, and some agricultural chemicals is easily absorbed by plants so that the pesticide volume of vegetable surface remaining is fewer, can not represent agricultural chemicals
Total amount, the inaccurate problem of testing result.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme is described in further detail, but protection scope of the present invention is not
It is confined to the following stated.
The general aspects of Rogor: the molecular formula of Rogor is C5H12NO3PS2, it means that Rogor molecule contains a sulphur generation
Phosphate radical so that Sulfur capacity therein is easily electrolysed out sulphion in water so that it can react with silver nitrate, generates yellow mercury oxide；
React with palladium bichloride, generate yellow substance.
The reproducibility of Rogor: sulphion has stronger reproducibility, therefore can reduce some oxidizing chemicals, example
Such as Fe3+, potassium permanganate etc..
Rogor water-disintegrable: Rogor in neutral conditions can hydrolysis methylamine, react with DNFB, produce Huang
Look precipitates.In the basic conditions, can react with natrium nitroferrocyanatum, produce reddish-brown precipitation.
Fluorescence method: owing to Rogor itself is without fluorescence, the present invention attempted FITC, salicyl fluorone dimer, two
The fluorescence colour of fluorescein stain is commonly used in the laboratories such as iodine fluorescein, calcein, it is intended to find out a kind of relatively reasonable detection
Means.
1.1 ordinary chemical methods:
At the test initial stage, after specifying object of experiment, start to set about from the chemical property that Rogor is most basic, it would be desirable to from common are
The chemical reaction of color change finds out the reagent that a kind of precision is higher.
1.1.1 direct reaction method
1.1.1.1 the basic chemical property of Rogor
At the initial stage, attempt this material of silver nitrate at first.Take the 40 percent Rogor emulsion being commercially available, with bottle label subscript
Bright 1:1000 dilution ratio is diluted in water.Owing to Rogor is slightly soluble in water, after dilution, Rogor emulsion can be with the form of droplet
Sink to beaker bottom, therefore take the method for ultrasonic vibration and stand 1H, Rogor emulsion is diffused in whole solution system so that it is
Even concentration, also substantially reduces the time of dissolving.Take the silver nitrate solution of the 0.5 milliliter of 1mol/L in laboratory in small test tube,
Add the Rogor aqueous solution 0.5 milliliter prepared, shake gently, stand 10min.Do not observe yellow mercury oxide, but solution has become
Obtain muddy.Analyze: one, simply present muddiness due to solution and the most obvious yellow mercury oxide, therefore by the method not
Can the most substantially observe result.Two, it is a kind of expensive salting liquid due to silver nitrate, if it is made as one high-volume
Detection method, do not meet the feature of Huimin, high cost.Institute's failure in this way.
Furthermore, attempted again this chemical substance of palladium bichloride, the same silver nitrate of method.After standing, it was observed that significantly yellow
Precipitate, and energy naked eyes clearly tell the color change of solution.Therefore consider further with filter paper as medium, use filter paper colorimetric
Method.But through inquiry, find that palladium is a kind of noble metal, have an indispensable effect in many high frontiers, and palladium element
Yield is the highest, and cost is the highest, therefore is not suitable for batch and uses.
After this, the present invention adds, for the chemical method of new try, the premise that a chemicals is conventional and cheap.
After continuously failure the most several times, it is contemplated that phosphate radical is unstable, there is the character of strong reducing property, in addition phosphate radical
One of them is the fact that oxonium ion is substituted by sulphion, has associated and has utilized the redox reaction having color to change to detect pleasure
The really method of molecule.
1.1.1.2 the redox reaction of Rogor
1) aqueous solution of ferric ion presents yellow, its be reduced after ion color fade.Take iron chloride powder
0.1625g, is dissolved in 10 milliliters of water, forms the ferric chloride in aqueous solution of 0.1mol/L, stands 30Min.0.5 milli of proportioning before taking
The liter Rogor aqueous solution, in small test tube, adds 0.5 milliliter of ferric chloride solution, concussion.Observing, yellow solution the most substantially becomes
Changing, after ultrasonic vibration 15MIN, yellow is slightly taken off, but observes and inconspicuous.So scheme failure.
2) potassium permanganate is a kind of strong oxidizer, and itself is with strong redness, if there is redox reaction, produces
Raw colourless divalent manganesetion, it will be easier to observe.Take the liquor potassic permanganate 1 of the good 1mol/L of laboratory proportioning
Milliliter, adds the Rogor aqueous solution 1 milliliter of 1:1000, shakes gently, finds that redness is substantially taken off, but creates what one was pungent
Gas, does not the most take notice of, and has begun to be immersed in liquor potassic permanganate filter paper and prepare next step experiment, but afterwards
Find after lookup data, if after eating Rogor by mistake, it is impossible to use potassium permanganate gastric lavage, because both meeting reactions generate a kind of poison
The material that property is more intensive.So scheme is contrary to the expection of " surveying poison ", scheme failure.
1.1.2 indirect reaction method
Before in view of indirect reaction method, the present invention have also been attempted many different chemical substances, but is substantially all with precision
Not high enough, the problems such as visual effect is the most obvious are excluded.Then, just whether chemical property in view of Rogor hydrolysate has
More practical detection method.
1.1.2.1 neutrallty condition
Rogor is the most relatively stable, does not hydrolyzes, and in neutral conditions, generates methylamine and 2,4-dinitro
The reaction of base chlorobenzene can generate yellow product.Seek pleasure the fruit aqueous solution 30 milliliters, use alkalescence the pH value of the Rogor aqueous solution adjusted to
8.00 left and right.Method: calibration PH meter, the fruit aqueous solution 30 milliliters of seeking pleasure, gos deep into liquid level by the probe that PH counts, puts into magnetite also simultaneously
Allow it work on mixing platform, use liquid-transfering gun to obtain the sodium hydroxide solution of 0.1mol/L, be dropwise slowly added into Rogor molten
In liquid, observing the numerical value change of PH meter, until stable about 8.00, regulation completes.
The Rogor solution left standstill 2H of PH will be regulated, take the Rogor solution 2 milliliters after standing, add 2 milliliters of proportionings good
DNFB.Observing, solution has gradually become faint yellow from water white transparency, but due to faint yellow can not be with the naked eye
Clearly differentiate, scheme failure.
1.1.2.2 alkalescence condition
Rogor is the most easily hydrolyzed into D2EHDTPA and mercaptan, sulfide and natrium nitroferrocyanatum reaction and generates ocean
Red compound.Seek pleasure fruit the aqueous solution 30 milliliters, with the PH control method of 3.1.2.1, solution PH is adjusted to about 10.00,
Stand 20min, take the Rogor solution 2 milliliters after standing, add the natrium nitroferrocyanatum solution 2 milliliters of 1mol/L.Observe,
Owing to natrium nitroferrocyanatum itself carries yellow green, after joining Rogor solution, become brick-red from yellow green at once, face
Discolorationization is the most obvious.Observing, this material is possible as the coloring agent of test paper method, but contrasts reality when going to second time
The when of testing, find that the natrium nitroferrocyanatum solution of firm proportioning occurs in that blue attachment on wall of cup, and yellow green is bright
Aobvious being converted to light blue, learnt by data afterwards, the aqueous solution of natrium nitroferrocyanatum is the material of a kind of extremely unstable, in room
Under the conditions of temperature will fast decoupled, scheme failure.
1.2 fluorescence method
Through above-mentioned many experiments, the direct reaction method of color chemicals seems and does not reaches the precision required for detection.
1.2.1 direct staining method
Based on fluorescence colour, the present invention has attempted the dye test of multiple fluorescent substance.
1.2.1 salicyl fluorone
Salicyl fluorone is a kind of reagents for anion, has the strongest fluorescence in neutral conditions, and it can be cloudy with many
Property ions binding, thus reduce fluorescence intensity.Utilizing this feature, the present invention attempts using it directly to dye Rogor through row,
Owing to Rogor can ionize out anionic radical in water, in theory, after dyeing terminates, its fluorescence intensity should be able to decline.
Method:
Taking 40 percent Rogor solution, according to the dilution proportion of 1:1000, the Rogor aqueous solution being configured to 50 milliliters is stand-by.Take
Laboratory salicyl fluorone powder, weighs with assay balance, according to the molecular weight demarcated on bottle, is configured to the molten of 0.5mol/L
Liquid is stand-by.Take the salicyl fluorone 2 milliliters configured in test tube, add 2 milliliters of Rogor solution, be placed on water bath with thermostatic control and add
Hot stove reacts, and duration is about 2H.
Result is observed:
Salicyl fluorone itself presents yellow green, and after adding Rogor solution, yellow is thin out, by dilute for the ketone deionized water of equivalent
After releasing, observing little with the solution gap containing Rogor, therefore can determine whether, there is not violent chemical reaction in the initial stage both.
After heating water bath 2H, former yellow-green soln is found to have red appearance slightly the most afterwards, but inconspicuous, through the purple in darkroom
Outer lamp, finds that fluorescence intensity weakens.
Analyze:
1. salicyl fluorone can react with Rogor really so that it is fluorescence takes off.
2. it is relatively complicated with the condition that Rogor reacts, and needs the overlong time consumed.
3., by above-mentioned experiment, because the reaction time is long, can not conclude that Rogor causes the fluorescence of ketone and subtracts completely
Weak, it is also possible to the decomposition being own causes the illusion of change in fluorescence.So scheme is not passed through.
1.2.2 indirect fluorescent detection method
Process based on above-mentioned experiment think deeply, the method that the present invention is considered be substantially " xxxxx reacts with Rogor, generation
XXXXX, causes color or fluorescence intensity to change ", it is clear that this mode of thinking has been limited to finding a kind of suitableization on certain
Learn the direction of material.In the face of a lot of unknown things, people often select to go to solve by aspectant mode, and this is greatly certainly
In the case of part or set up, but for some things, some field, find a kind of intermediate and resolve contradiction both sides' meeting
More effective, such as, space probation, deep-sea exploration, drug study, building simulation etc..These are by by hardware, software etc.
The method indirectly exploring tera incognita so that the mankind have entered the unprecedented knowledge explosion epoch since 19th century, we
Our eyes can be replaced by program, replace our strength with machinery, complete many human bodies and can not complete or can not be real
In existing field, this research mode by the third party, our New World of pioneer.
By the process of these emerging technology exploration discoveries, associate the obstruction of Rogor experiment, the most just in view of this
The bright mode that whether can get involved with a kind of third party, must couple together more effective for both chemical property.
Probing into and obtain, this fluorescent material of calcein is the most extremely stable, and it is mainly used to titration calcium element,
Can also be used for measuring strontium, barium, copper, manganese, cobalt, nickel, molybdenum, chromium etc..It has powerful gravitation for some metal cation, and
Obviously, after being combined with these metal ions, its fluorescence intensity can substantially weaken, and the yellow green of solution itself also can be taken off.Due to
May be used for titration, the sensitivity of this fluorescent material and Precision Theory can reach requirement of experiment.
Due to Rogor solution instability under alkaline environment, stable in acid condition, Rogor molecule itself can be obtained
The positive relatively strong, then the present invention through went by calcein and Rogor solution directly in conjunction with mode, but effect is barely satisfactory.
Put problem before eyes to have:
1) a kind of material can be found so that " calcein XXXX this material Rogor solution " this reactive mode
Produce obvious result.
2) this material can react with calcein, can react with Rogor again simultaneously.
3) result that reaction produces can have higher precision and sensitivity.
With these three problem, start with from the material that can react with calcein at first.
First, those positive ions are got rid of, it is clear that these positive ions can't send out into strong chemistry with Rogor
Reaction.
Furthermore, those materials with calcein generation altered chemical structure are also got rid of, because, if thisization
Learning material and result in the disappearance of fluorescent material, if Rogor still can react with it, can not determine the end in theory is that Rogor creates
Result or this reactive material creates result.
Finally, the present invention, from surfactant, examines whether to exist a kind of activating agent, can with calcein and
Rogor combines, but the tightst with the combination of Rogor and strong.
The organophosphorus pesticide Determination of Dimethoate Residues detection method that [embodiment 1] chromatographs based on silica gel plate, comprises the following steps:
S1: preparation detection liquid, including following sub-step:
S101: prepare original solution:
(1) take 0.429 gram of calcein powder, be dissolved in 50 milliliters of water, be configured to the calcein solution that concentration is 1mol/L；
(2) taking 0.247 gram of cetyl trimethylammonium bromide powder, be dissolved in 50 ml deionized water, being configured to concentration is
The cetyl trimethylammonium bromide solution of 0.5mol/L；
S102: be the ratio of 1:2 according to volume ratio, by molten with cetyl trimethylammonium bromide for the calcein solution configured
Liquid mixes, and concussion obtains detecting liquid gently；
S2: colorimetric detection, including following sub-step:
S201: use tlc silica gel plate, smashs liquid to pieces in its one end instillation target to be measured and chromatographs；
S202: after chromatography is complete, instills some farthest in distance and instills the detection liquid obtained by step S1；
S203: be placed in darkroom by silica gel plate and irradiate with ultraviolet light, observes and drips whether there is obvious yellow-green fluorescence at detection liquid
Produce, if there being obvious yellow-green fluorescence to produce, having excessive organophosphorus pesticide Determination of Dimethoate Residues, otherwise then there is no excessive organophosphor
Agricultural chemicals Determination of Dimethoate Residues.
The organophosphorus pesticide Determination of Dimethoate Residues detection method that [embodiment 2] chromatographs based on silica gel plate, comprises the following steps:
S1: preparation detection liquid, including following sub-step:
S101: prepare original solution:
(1) calcein powder is taken, soluble in water, it is configured to the calcein solution that concentration is 0.05mol/L；
(2) take cetyl trimethylammonium bromide powder, be dissolved in deionized water, be configured to that concentration is 0.025mol/L 16
Alkyl trimethyl ammonium bromide solution；
S102: be the ratio of 1:2 according to volume ratio, by molten with cetyl trimethylammonium bromide for the calcein solution configured
Liquid mixes, and concussion obtains detecting liquid gently；
S2: colorimetric detection, including following sub-step:
S201: use tlc silica gel plate, smashs liquid to pieces in its one end instillation target to be measured and chromatographs；
S202: after chromatography is complete, instills some farthest and without being respectively dropped into the inspection obtained by step S1 at chromatography in distance
Survey liquid；
S203: observe and whether have obvious color distortion at above-mentioned two, if there being obvious color distortion, has excessive organophosphor agriculture
Medicine Determination of Dimethoate Residues, on the contrary then there is no excessive organophosphorus pesticide Determination of Dimethoate Residues.
The organophosphorus pesticide Determination of Dimethoate Residues detection method that [embodiment 3] chromatographs based on silica gel plate, comprises the following steps:
S1: preparation detection liquid, including following sub-step:
S101: prepare original solution:
(1) calcein powder is taken, soluble in water, it is configured to the calcein solution that concentration is 0.1mol/L；
(2) take cetyl trimethylammonium bromide powder, be dissolved in deionized water, be configured to the hexadecane that concentration is 0.1mol/L
Base trimethylammonium bromide solution；
S102: be the ratio of 1:2 according to volume ratio, by molten with cetyl trimethylammonium bromide for the calcein solution configured
Liquid mixes, and concussion obtains detecting liquid gently；
S2: colorimetric detection, including following sub-step:
S201: use tlc silica gel plate, smashs liquid to pieces in its one end instillation target to be measured and chromatographs；
S202: after chromatography is complete, instills some farthest in distance and instills the detection liquid obtained by step S1；
S203: be placed in darkroom by silica gel plate and irradiate with ultraviolet light, observes and drips whether there is obvious yellow-green fluorescence at detection liquid
Produce, if there being obvious yellow-green fluorescence to produce, having excessive organophosphorus pesticide Determination of Dimethoate Residues, otherwise then there is no excessive organophosphor
Agricultural chemicals Determination of Dimethoate Residues.
Laboratory result
The core thinking of indirect fluorescent method is: this by " a kind of fluorescent material----certain intermediate medium----Determination of Dimethoate Residues "
Mode detects the existence of Determination of Dimethoate Residues.Configuration compound concentration: calcein (0.1mol/L), CTMAB (0.1mol/L),
Rogor solution (1:1000 dilution).
Test in order to more reasonability must explore the result obtained, it is intended to find out the most rational concentration proportioning.
1) calcein excess
Take the calcein solution 1ml configured in 5 test tubes, be separately added into 0.1mol/L, 0.05mol/L, 0.025mol/
The CTMAB solution 1ml of L, 0.0125mol/L, 0.00625mol/L, observes the change of fluorescence intensity, observes,
After the magnitude of 0.025mol/L, fluorescence intensity is without significant change, therefore taking 0.025mol/L is zero dividing value, by 0.025mol/L with
0.1mol/L compares, and the effect obtaining 0.1mol/L is better than 0.025mol/L.
2) CTMAB excess
Take the CTMAB solution 1ml configured in 5 test tubes, be separately added into 0.1mol/L, 0.05mol/L, 0.025mol/L,
The calcein solution 1ml of 0.0125mol/L, 0.00625mol/L, observes the change of fluorescence intensity, observes,
After the magnitude of 0.05mol/L, fluorescence intensity is without significant change, therefore taking 0.05mol/L is zero dividing value, by 0.05mol/L with
0.1mol/L contrasts, and the effect obtaining 0.1mol/L is better than 0.05mol/L.
Therefore, to be about effect when of 1 to 1 best for calcein and the ratio of CTMAB.
The above is only the preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein
Form, is not to be taken as the eliminating to other embodiments, and can be used for other combinations various, amendment and environment, and can be at this
In the described contemplated scope of literary composition, it is modified by above-mentioned teaching or the technology of association area or knowledge.And those skilled in the art are entered
The change of row and change, the most all should be at the protection domains of claims of the present invention without departing from the spirit and scope of the present invention
In.
Claims (6)
1. organophosphorus pesticide Determination of Dimethoate Residues detection method based on silica gel plate chromatography, it is characterised in that comprise the following steps:
S1: preparation detection liquid, including following sub-step:
S101: prepare original solution:
(1) take calcein powder, be dissolved in the first solvent, be configured to the concentration calcein not less than 0.05 mol/L molten
Liquid；
(2) take cetyl trimethylammonium bromide powder, be dissolved in the second solvent, be configured to concentration not less than 0.025mol/L's
Cetyl trimethylammonium bromide solution；
S102: be the ratio of 1:2 according to volume ratio, by molten with cetyl trimethylammonium bromide for the calcein solution configured
Liquid mixes, and concussion obtains detecting liquid gently；
S2: colorimetric detection, including following sub-step:
S201: use tlc silica gel plate, smashs liquid to pieces in its one end instillation target to be measured and chromatographs；
S202: after chromatography is complete, instills some farthest in distance and instills the detection liquid obtained by step S1；
S203: be placed in darkroom by silica gel plate and irradiate with ultraviolet light, observes and drips whether there is obvious yellow-green fluorescence at detection liquid
Produce, if there being obvious yellow-green fluorescence to produce, having excessive organophosphorus pesticide Determination of Dimethoate Residues, otherwise then there is no excessive organophosphor
Agricultural chemicals Determination of Dimethoate Residues.
Organophosphorus pesticide Determination of Dimethoate Residues detection method based on silica gel plate chromatography the most according to claim 1, its feature exists
In: the concentration of described calcein solution is 1mol/L, and the concentration of described cetyl trimethylammonium bromide solution is 0.5mol/
L。
Organophosphorus pesticide Determination of Dimethoate Residues detection method based on silica gel plate chromatography the most according to claim 2, its feature exists
In: described calcein solution is 1:2 with the volume ratio of described cetyl trimethylammonium bromide solution.
Organophosphorus pesticide Determination of Dimethoate Residues detection method based on silica gel plate chromatography the most according to claim 1, its feature exists
In: the first described solvent is water.
Organophosphorus pesticide Determination of Dimethoate Residues detection method based on silica gel plate chromatography the most according to claim 1, its feature exists
In: the second described solvent is deionized water.
6. organophosphorus pesticide Determination of Dimethoate Residues detection method based on silica gel plate chromatography, it is characterised in that comprise the following steps:
S1: preparation detection liquid, including following sub-step:
S101: prepare original solution:
(1) take calcein powder, be dissolved in the first solvent, be configured to the concentration calcein not less than 0.05 mol/L molten
Liquid；
(2) take cetyl trimethylammonium bromide powder, be dissolved in the second solvent, be configured to concentration not less than 0.025mol/L's
Cetyl trimethylammonium bromide solution；
S102: be the ratio of 1:2 according to volume ratio, by molten with cetyl trimethylammonium bromide for the calcein solution configured
Liquid mixes, and concussion obtains detecting liquid gently；
S2: colorimetric detection, including following sub-step:
S201: use tlc silica gel plate, smashs liquid to pieces in its one end instillation target to be measured and chromatographs；
S202: after chromatography is complete, instills some farthest and without being respectively dropped into the inspection obtained by step S1 at chromatography in distance
Survey liquid；
S203: observe and whether have obvious color distortion at above-mentioned two, if there being obvious color distortion, has excessive organophosphor agriculture
Medicine Determination of Dimethoate Residues, on the contrary then there is no excessive organophosphorus pesticide Determination of Dimethoate Residues.
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| CN109425675A (en) * | 2017-08-22 | 2019-03-05 | 深圳市美信分析技术有限公司 | A kind of method of Organophosphorus Pesticide Residues diazinon in vegetables by HPLC |
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| CN109425675A (en) * | 2017-08-22 | 2019-03-05 | 深圳市美信分析技术有限公司 | A kind of method of Organophosphorus Pesticide Residues diazinon in vegetables by HPLC |
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