18种除草剂中有效成分含量检测方案

Experimental Details Data Processing Kristina Kirkham， Luisa Pereira， Derek Hillbeck， Thermo Fisher Scientific， Runcorn，UK Accucore Vanquish， Vanquish UHPLC， pesticides， herbicides， rapidseparation， high resolution Abstract This application shows the advantages of using the Thermo ScientificTMAccucoreTM VanquishTM C18 1.5 pm UHPLC column and the VanquishUHPLC system for the separation of 18 herbicides. The advancedcapabilities of the Vanquish UHPLC system allow the Accucore Vanquishcolumns to be operated at higher flow rates that enable development ofrapid， high-performance analytical methods. Comparisons are made withother commercially available sub-2 pm solid core columns， demonstratingimproved peak capacity and resolution. system and the low dispersion Thermo ScientificTMDionexTM ViperTM fingertight fitting capillaries allow theuser to take full advantage of the separation power of theAccucore Vanquish UHPLC column. The 1500 barpressure capability of the Vanquish pump enables anextended range of flow rates to be employed allowing forfaster separations and higher throughput. Consumables Part Number Accucore Vanquish C18 1.5 pm UHPLC column， 100×2.1 mm 17101-102130 Fisher ScientificTM HPLC grade water 10221712 Fisher Scientific HPLC grade acetonitrile 10616653 Thermo ScientificTM VirtuosoTM 9 mm wide opening， 2 mL screw thread vial and cap kit 60180-VT400(recommended) Sample Preparation Pesticide mix 18 obtained from Neochema (Bodenheim/Manz， Germany) containing the following pesticides at 10 pg/mLin acetonitrile： (1) desethylatrazine， (2) metoxuron， (3) hexazinone， (4) simazine， (5) cyanazine， (6) methabenzthiazuron，(7)chlorotoluron， (8) atrazine， (9) monolinuron， (10) diuron， (11) isoproturon， (12) metobromuron， (13) metazachlor， (14) sebuthylazin， (15) propazine， (16) terbuthylazine， (17) linuron， (18) metolachlor Sample was diluted 1：1 with water to produce a working solution with a 5 pg/mL concentration Instrumentation Part Number Vanquish UHPLC system consisting of： Binary pump H VH-P10-A Split sampler HT VH-A10-A Column compartment H VH-C10-A Diode array detector HL VH-D10-A Thermo ScientificTM VirtuosoTM Vial Identification System 60180-VT-100 Separation Conditions Mobile phase A： Water Mobile phase B： Acetonitrile Column temperature： 43°℃ Injection details： 0.5 pL Detection： UV at 230 nm (0.1 s rise time， 50 Hz， 8 nm slit width) UHPLC Column 1： Accucore Vanquish C18 1.5 um， 100×2.1 mm Flow rate： 0.65 mL/min Time (min) %A %B 0.00 80 20 4.00 60 40 7.00 20 80 7.50 80 20 12.00 80 20 Table 1： Gradient conditions for the Accucore Vanquish 1.5 um and competitor columns (i) and (ii) UHPLC Column 2： Solid core C18 2.6 um， 100 x2.1 mm Flow Rate： 0.38 mL/min Time (min) %A %B 0.00 80 20 6.93 60 40 12.13 20 80 13.00 80 20 20.80 80 20 Table 2： Gradient conditions for the 2.6 um solid core column Software： Thermo ScientificTM DionexTM ChromeleonTM 7.2 Chromatography Data System (CDS) Results A comparative study of the Accucore Vanquish 1.5 pm and sub-2 pm competitor columns wascarried out using the same herbicide mixture and chromatographic method with a flow rate of0.65 mL/min and a two-stage binary gradient from 20% to 80% acetonitrile over 7 minutes.Baseline separation of 16 out of 18 compounds was achieved on all columns in less than 6 minutes(Figure 1). Time (min) Figure 1： Chromatographic separation of eighteen herbicides on Accucore Vanquish UHPLC column (black)，competitor (i) (blue) and competitor (ii) (purple) columns The Accucore Vanquish UHPLC column demonstrated superior performance with averagepeak widths 21% and 60% lower (Figure 2) than competitor (i) and (ii)， respectively. As a consequence peak capacity was 17% higher than competitor (i) and 37%higher thancompetitor (ii). M Accucore Vanquish ■Competitor (i) ■ Competitor (il) Figure 2： Comparison of peak widths for the Accucore Vanquish UHPLC column (black)， competitor (i) (blue) andcompetitor (ii) (purple) columns. Peaks 10 and 11 coelute on competitor columns (i) and (ii). Overall， average resolution on the Accucore Vanquish UHPLC column was 6% and 31% greaterthan that achieved by competitor (i) and (ii)， respectively (Figure 3). Peak heights were 11% and23% higher than competitor (i) and (ii)， respectively (Figure 4). In addition， the Accucore Vanquishcolumn was less retentive with average retention times being 3% and 5% lower than those oncompetitor (i) and (ii)(Figure 5). 30- ■Accucore Vanquish ■Competitor (i) ■ Competitor (ii) Figure 3： Comparison of resolution between the Accucore Vanquish UHPLC column (black)， competitor (i) (blue)and competitor (ii) (purple) columns. Peaks 10 and 11 coelute on competitor columns (i) and (ii). Figure 4： Comparison of peak height on the Accucore Vanquish UHPLC column (black)， competitor (i) (blue) andcompetitor (ii) (purple) columns. Peaks 10 and 11 coelute on competitor columns (i) and (ii). mAccucore Vanquish ■Competitor (i) ■Competitor (ii) Figure 5： Comparison of retention times on the Accucore Vanquish UHPLC column (black)， competitor (i) (blue)and competitor (ii) (purple) columns. Peaks 10 and 11 coelute on competitor columns (i) and (ii). The chromatographic data shown in Figure 6 and subsequent figures demonstrate the advantagesof scaling a method from a 2.6 um solid core column to the Accucore Vanquish 1.5 pm UHPLCcolumn. The separation of 18 herbicides was achieved 40% faster on the Accucore Vanquish1.5 um UHPLC column used in conjunction with the Vanquish UHPLC system. Figure 6： Chromatographic separation of 18 herbicides on a 2.6 um solid core column (top) and the AccucoreVanquish UHPLC column (bottom) In addition，peak widths were reduced by 56%， peak heights were improved by 17% (Figure 7)，peak capacity was improved by 31%， and， as a result， average resolution was improved by 24%(Figure 8). ■Accucore Vanquish 1.5 um Solid Core 2.6 um Figure 7： Comparison of peak height between the Accucore Vanquish UHPLC column and a 2.6 um solid corecolumn 30- ■Accucore Vanquish 1.5 pmSolid Core 2.6 um Figure 8： Comparison of resolution between the Accucore Vanquish UHPLC column and a 2.6 pm solid corecolumn Conclusion This application demonstrates the advantages of using the Accucore Vanquish C18 1.5 pm UHPLCcolumn and Vanquish UHPLC system for the analysis of herbicides. The solution deliversseparation of 18 herbicides in less than 6 minutes. When compared to competitor sub-2 um solid core columns it delivers： ●Greater peak capacity Increased resolution Increased sensitivity When compared to a solid core 2.6 um particle packed column it delivers： Reduced analysis time ●Increased resolution Improved sensitivity Greater peak capacity thermoscientific.com/accucore C 2014 Thermo Fisher Scientific Inc. All rights reserved. All trademarks are the property of Thermo Fisher Scientific and its subsidiaries. This information ispresented as an example of the capabilities of Thermo Fisher Scientific products. It is not intended to encourage use of these products in any manners that mightinfringe the intellectual property rights of others. Specifications， terms and pricing are subject to change. Not all products are available in all countries.Please consult your local sales representative for details. 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