CN105241983B - 一种用于食品中农药残留检测的色谱柱 - Google Patents
一种用于食品中农药残留检测的色谱柱 Download PDFInfo
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- CN105241983B CN105241983B CN201510638012.1A CN201510638012A CN105241983B CN 105241983 B CN105241983 B CN 105241983B CN 201510638012 A CN201510638012 A CN 201510638012A CN 105241983 B CN105241983 B CN 105241983B
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- cyclodextrin
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- chromatographic column
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- pesticide residues
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- 239000000447 pesticide residue Substances 0.000 title claims abstract description 11
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 8
- 239000000178 monomer Substances 0.000 claims abstract description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 239000010453 quartz Substances 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000001257 hydrogen Substances 0.000 claims abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 13
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- XJUZRXYOEPSWMB-UHFFFAOYSA-N Chloromethyl methyl ether Chemical compound COCCl XJUZRXYOEPSWMB-UHFFFAOYSA-N 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 229940061627 chloromethyl methyl ether Drugs 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000012670 alkaline solution Substances 0.000 claims description 2
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000032683 aging Effects 0.000 claims 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- 239000004593 Epoxy Substances 0.000 claims 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 238000013019 agitation Methods 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 125000001033 ether group Chemical group 0.000 claims 1
- 238000009413 insulation Methods 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 229920001296 polysiloxane Polymers 0.000 claims 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 239000013049 sediment Substances 0.000 claims 1
- 238000006467 substitution reaction Methods 0.000 claims 1
- 235000013305 food Nutrition 0.000 abstract description 9
- 238000001514 detection method Methods 0.000 abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 6
- 238000004817 gas chromatography Methods 0.000 abstract description 5
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 abstract description 4
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 abstract description 3
- 235000013339 cereals Nutrition 0.000 abstract description 2
- 235000013399 edible fruits Nutrition 0.000 abstract description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 abstract description 2
- 235000013311 vegetables Nutrition 0.000 abstract description 2
- 239000006228 supernatant Substances 0.000 abstract 2
- 241000219112 Cucumis Species 0.000 abstract 1
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 abstract 1
- 230000005526 G1 to G0 transition Effects 0.000 description 12
- 238000006266 etherification reaction Methods 0.000 description 6
- 239000000575 pesticide Substances 0.000 description 6
- 238000006068 polycondensation reaction Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 235000018645 Allium odorum Nutrition 0.000 description 2
- 240000008654 Allium ramosum Species 0.000 description 2
- 235000005338 Allium tuberosum Nutrition 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000007306 functionalization reaction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 239000002917 insecticide Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002728 pyrethroid Substances 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BLSQLHNBWJLIBQ-OZXSUGGESA-N (2R,4S)-terconazole Chemical compound C1CN(C(C)C)CCN1C(C=C1)=CC=C1OC[C@@H]1O[C@@](CN2N=CN=C2)(C=2C(=CC(Cl)=CC=2)Cl)OC1 BLSQLHNBWJLIBQ-OZXSUGGESA-N 0.000 description 1
- WURBVZBTWMNKQT-UHFFFAOYSA-N 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butan-2-one Chemical compound C1=NC=NN1C(C(=O)C(C)(C)C)OC1=CC=C(Cl)C=C1 WURBVZBTWMNKQT-UHFFFAOYSA-N 0.000 description 1
- PXMNMQRDXWABCY-UHFFFAOYSA-N 1-(4-chlorophenyl)-4,4-dimethyl-3-(1H-1,2,4-triazol-1-ylmethyl)pentan-3-ol Chemical compound C1=NC=NN1CC(O)(C(C)(C)C)CCC1=CC=C(Cl)C=C1 PXMNMQRDXWABCY-UHFFFAOYSA-N 0.000 description 1
- SYOANZBNGDEJFH-UHFFFAOYSA-N 2,5-dihydro-1h-triazole Chemical compound C1NNN=C1 SYOANZBNGDEJFH-UHFFFAOYSA-N 0.000 description 1
- GOCUAJYOYBLQRH-UHFFFAOYSA-N 2-(4-{[3-chloro-5-(trifluoromethyl)pyridin-2-yl]oxy}phenoxy)propanoic acid Chemical compound C1=CC(OC(C)C(O)=O)=CC=C1OC1=NC=C(C(F)(F)F)C=C1Cl GOCUAJYOYBLQRH-UHFFFAOYSA-N 0.000 description 1
- YUVKUEAFAVKILW-UHFFFAOYSA-N 2-(4-{[5-(trifluoromethyl)pyridin-2-yl]oxy}phenoxy)propanoic acid Chemical compound C1=CC(OC(C)C(O)=O)=CC=C1OC1=CC=C(C(F)(F)F)C=N1 YUVKUEAFAVKILW-UHFFFAOYSA-N 0.000 description 1
- ABOOPXYCKNFDNJ-UHFFFAOYSA-N 2-{4-[(6-chloroquinoxalin-2-yl)oxy]phenoxy}propanoic acid Chemical compound C1=CC(OC(C)C(O)=O)=CC=C1OC1=CN=C(C=C(Cl)C=C2)C2=N1 ABOOPXYCKNFDNJ-UHFFFAOYSA-N 0.000 description 1
- HOSGXJWQVBHGLT-UHFFFAOYSA-N 6-hydroxy-3,4-dihydro-1h-quinolin-2-one Chemical group N1C(=O)CCC2=CC(O)=CC=C21 HOSGXJWQVBHGLT-UHFFFAOYSA-N 0.000 description 1
- 0 C*CC1CCC(C*)CC1 Chemical compound C*CC1CCC(C*)CC1 0.000 description 1
- 239000005946 Cypermethrin Substances 0.000 description 1
- 239000001116 FEMA 4028 Substances 0.000 description 1
- 239000005839 Tebuconazole Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 235000011175 beta-cyclodextrine Nutrition 0.000 description 1
- 229960004853 betadex Drugs 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- ZXQYGBMAQZUVMI-UNOMPAQXSA-N cyhalothrin Chemical compound CC1(C)C(\C=C(/Cl)C(F)(F)F)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-UNOMPAQXSA-N 0.000 description 1
- 229960005424 cypermethrin Drugs 0.000 description 1
- KAATUXNTWXVJKI-UHFFFAOYSA-N cypermethrin Chemical compound CC1(C)C(C=C(Cl)Cl)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 KAATUXNTWXVJKI-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- VMGAPWLDMVPYIA-HIDZBRGKSA-N n'-amino-n-iminomethanimidamide Chemical compound N\N=C\N=N VMGAPWLDMVPYIA-HIDZBRGKSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- QIIPQYDSKRYMFG-UHFFFAOYSA-N phenyl hydrogen carbonate Chemical compound OC(=O)OC1=CC=CC=C1 QIIPQYDSKRYMFG-UHFFFAOYSA-N 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- BOLDJAUMGUJJKM-LSDHHAIUSA-N renifolin D Natural products CC(=C)[C@@H]1Cc2c(O)c(O)ccc2[C@H]1CC(=O)c3ccc(O)cc3O BOLDJAUMGUJJKM-LSDHHAIUSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229960000580 terconazole Drugs 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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CN201510638012.1A CN105241983B (zh) | 2015-09-30 | 2015-09-30 | 一种用于食品中农药残留检测的色谱柱 |
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CN201510638012.1A CN105241983B (zh) | 2015-09-30 | 2015-09-30 | 一种用于食品中农药残留检测的色谱柱 |
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CN105241983B true CN105241983B (zh) | 2017-07-14 |
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CN108398506B (zh) * | 2018-04-11 | 2020-02-04 | 国家烟草质量监督检验中心 | 一种超高效合相色谱-串联质谱技术拆分、测定手性农药喹禾灵和吡氟禾草灵对映体的方法 |
CN112378723A (zh) * | 2020-11-19 | 2021-02-19 | 深圳市易瑞生物技术股份有限公司 | 一种用于分离和浓缩目标物的样品垫及其用途 |
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DE4317139A1 (de) * | 1993-05-21 | 1994-11-24 | Volker Prof Dr Schurig | Verfahren zur präparativen gaschromatographischen Enantiomerentrennung von Inhalationsanästhektika (Enfluran) an Cyclodextrinderivaten in Polysiloxanlösung |
US20050106068A1 (en) * | 2003-11-18 | 2005-05-19 | Abdul Malik | Sol-gel dendron separation and extraction capillary column |
JP4417161B2 (ja) * | 2004-04-07 | 2010-02-17 | 長谷川香料株式会社 | 置換シクロデキストリンおよびその製法 |
JP2005344034A (ja) * | 2004-06-04 | 2005-12-15 | National Institute Of Advanced Industrial & Technology | シクロデキストリンを結合させた吸着材 |
JP2005031091A (ja) * | 2004-08-05 | 2005-02-03 | T Hasegawa Co Ltd | ガスクロマトグラフィー用光学活性カラム充填剤 |
CN101015789A (zh) * | 2007-01-05 | 2007-08-15 | 中国农业大学 | 新型β-环糊精衍生物毛细管气相色谱手性固定相及其制备方法 |
CN102649049B (zh) * | 2011-02-23 | 2014-06-11 | 中国农业科学院植物保护研究所 | 2,3-二-O-甲氧甲基-6-O-苄基-β-环糊精气相色谱手性固定相及其制备方法 |
CN102768250B (zh) * | 2012-07-23 | 2014-02-12 | 中国农业大学 | 毛细管气相色谱手性分离测定乳酸甲酯光学异构体的方法 |
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Inventor after: Zhao Linping Inventor after: Yu Qingwei Inventor after: Zhang Jie Inventor after: Miao Yinping Inventor after: Wu Zhijian Inventor after: Wei Zhuo Inventor before: Zhao Linping |
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Effective date of registration: 20170605 Address after: 450000 science Avenue, Henan, Zhengzhou, No. 100 Applicant after: Zhengzhou University Applicant after: Zhengzhou Zhongdao Biological Technology Co., Ltd. Address before: 450000 science Avenue, Henan, Zhengzhou, No. 100 Applicant before: Zhao Linping |
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