SPE Column for Pesticides Analysis
Solid phase extraction (SPE) column for pesticide analysis, "Presep® Agri series", is a cartridge packed with styrene divinylbenzene-methacrylate to clean up residual pesticides easily. Two types available depending on clean-up methods (pressure method or vacuum method): Presep®-C Agri (Short) cartridge with both ends closed and Presep® Agri syringe.
Features
- Ideal to concentrate hydrophobic trace substances in water samples.
- High recovery rate in pesticides even in polar metal coordinating compounds such as Ashram and oxine copper.
- Rapid processing with vacuum concentrators and pressurized flow pump for collection and concentration.
- A combination of Wakopak® Wakosil® Agri-9 and special eluent enables a easy and quick HPLC analysis of various pesticides.
- GC analysis can be carried out in high selectivity using Trajan (SGE) capillary columns.
Analytical Example (LC-MS/MS)
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Column:Presep®-C Agri (Short)
pre-conditioning for column
① CH3CN 10 mL
② CH3OH 10mL
③ H2O 10mL
1) flow sample water: 500 mL*1
2) washing: H2O 5 mL
3) extraction by CH3CN 2 mL
4) concentrate (to 0.2〜0.3 mL) under N2
5) dissolve into 1mL of H2O
6) analysis by HPLC (10 μL injection)*1 500 mL of sample: add 10 mL of 0.2 mol/L EDTA・2Na, pH3.5 by diluted HNO3 (conc.HNO3/H2O=1/10)
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HPLC conditions
Column : Wakopak® MS-Agri-9 GT (2.0 mmφ x 150 mm) Eluent : A)10 mM CH3COONH4 (pH3.7)
B)CH3CN
0-10min.: B=12-70 %
10-13min.: B=100 %
13-23min.: B=12 %Flow Rate :0.2 mL/min. at 40 ℃ Injection Vol. :each 1 ppm、2 μL MS/MS conditions
ESI, MRM
Ion Spray Voltage: 5500V (pos) -4500V (neg) Temperature: 700 ℃ 300 ℃ Curtain Gas: 40 20 Collision Gas: 5 3 Ion Source Gas1: 80 40 Ion Source Gas2: 70 80 System: 3200Q TRAP(ABI)
Results
18 components at positive mode
No.*1 | Chemical Name | Q1/Q3 | RT (min) | Recovery Rate (%) |
---|---|---|---|---|
74 | Methomyl | 163.1/88.1 amu | 4.4 | 50.8 (85.2)*2 |
71 | MPP oxon sulfoxide | 279.0/104.2 amu | 5.8 | 101.6 |
87 | Tricyclazole | 190.0/163.2 amu | 6.9 | 99.1 |
71 | MPP oxon sulfone | 295.0/217.1 amu | 7.2 | 99.7 |
18 | Carbofuran (metabolite of Carbosulfan) | 222.1/165.2 amu | 8.5 | 103.1 |
96 | Thiodicarb | 355.1/88.1 amu | 8.6 | 99.6 |
71 | MPP sulfoxide | 294.9/109.0 amu | 9.0 | 100.1 |
1 | Thiuram | 240.9/88.1 amu | 9.5 | 94.3 |
82 | Probenazole | 224.0/130.2 amu | 9.5 | 98.6 |
71 | MPP oxon | 263.0/231.1 amu | 9.6 | 99.5 |
86 | Bensulfuron-methyl | 411.0/149.2 amu | 10.0 | 100.7 |
95 | Flazasulfuron | 408.2/182.1 amu | 10.1 | 98.6 |
71 | MPP sulfone | 310.9/124.9 amu | 10.4 | 99.2 |
98 | Siduron peak1 | 233.1/137.2 amu | 10.4 | 99.7 |
98 | Siduron peak2 | - | 10.6 | 98.3 |
90 | Azoxystrobin | 404.1/372.1 amu | 10.8 | 99.6 |
84 | Dymron | 269.1/151.1 amu | 11.1 | 99.6 |
71 | MPP | 279.0/169.0 amu | 12.1 | 104.3 |
58 | Carpropamid | 336.0/139.2 amu | 12.2 | 101.8 |
*1 same number as Japanese Waterworks Act, Appendix.
*2 figure in parentheses is recovery rate when Presep® Agri was employed.
10 components at negative mode
No.*1 | Chemical Name | Q1/Q3 | RT (min) | Recovery Rate (%) |
---|---|---|---|---|
36 | Asulam | 228.9/196.7 amu | 5.7 | 99.6 |
17 | Bentazone | 239.1/131.6 amu | 6.8 | 99.3 |
19 | 2,4-PA | 219.9/161.7 amu | 7.5 | 99.1 |
20 | Triclopyr | 255.9/198.1 amu | 8.0 | 101.2 |
45 | MCPP(Mecoprop) | 213.0/140.9 amu | 8.8 | 99.9 |
94 | Halosulfuron-methyl | 433.6/252.2 amu | 9.6 | 99.1 |
68 | DCMU(Diuron) | 232.0/186.9 amu | 9.7 | 100.4 |
26 | Iprodione | 329.9/245.1 amu | 11.4 | 98.9 |
42 | Bensulide(SAP) | 395.9/212.7 amu | 12.3 | 96.7 |
102 | Fipronil | 436.8/330.1 amu | 12.4 | 97.3 |
*1 same number as Japanese Waterworks Act, Appendix.
Other 3 components without mixing*3
No.*1 | Chemical Name | Recovery Rate (%) |
---|---|---|
28 | Oxine-copper | 96.2 |
48 | Carbary (l NAC) | 101.0 |
75 | MBC (decomposition product of Benomyl) | 97.5 |
*1 same number as Japanese Waterworks Act, Appendix.
*3 due to stability in mixture solution.
Example by Presep®-C Agri (Short)
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SPE Conditions
Column :Presep®-C Agri (Short) Pre-conditioning :dichloromethane (5 mL), methanol (5 mL), DI water (5 mL) Sample :add 100 µL of standard solution into DI 200 mL of water SPE treatment :flow=10-20 mL/min. Draining :air flow for 10 min. Extraction and dryness :Attach two of Presep®-C Na2SO4 at the outlet and charge 2.5 mL of dichloromethane to extract. Then, remove Presep®-C Agri (Short) and Charge 6 mL of dichloromethane into Na2SO4 column. Combine crude solution. Concentration :add 2 mL of hexane and concentrate crude solution under N2 to ca. 0.8 mL (don't completely dryness). analytical sample :add 100 μL of internal standard solution and add 1 mL of hexane (sample solution should be in freezer to keep concentration due to vapolize). Standard :10 μg/mL acetone solution Internal standard solution :2 μg/mL of hexane solution with acenaphthene and chrysene (for adjusting agent for sensitivity of GC/MS analysis) GC conditions
GC : HP5890 PACKARD SERIESE GC/MS GC/MS : AUTO mass JMS-AM150 (JEOL) Column : 100 % dimethylpolysiloxane, 0.25 mmφ x 30 m, thickness=0.25 μm Injector : 250 ℃ Temp. : 60℃ (2min)-120℃ (20℃/min)-300℃(10℃/min)-300℃(5min) injection : 2.0 μL -
No. Chemical name Recovery rate (%) 27 etridiazole 92.3 30 chloroneb 91.8 33 pencycuron 90.8 43 benfluralin 82.3 2 simazine 101.5 10 propyzamide 95.8 9 TPN 95.8 6 diazinon 97.7 38 MBPMC 106.3 31 tolclofos-methyl 89.7 34 metalaxyl 100.7 7 MEP 97.3 37 dithiopyr 89.4 23 chlorpyrifos 88.9 29 captan 103.9 44 pendimethalin 85.7 46 methyldymron 84.6 22 isofenphos 91.3 8 isoprothiolane 96.6 41 butamifos 84.1 32 flutolanil 100.3 39 napropamide 99.7 5 isoxathion 91.8 triclopyr-2-butoxyethyl 94.1 35 mepronil 116.6 40 pyributicarb 93.5 26 iprodione 98.0 25 pyridaphenthion 106.5 11 DDVP(Dichlorvos) 108.9 12 BPMC 107.5 3 Thiobencarb 101.0 15 IBP 115.1 13 CNP 112.0 16 EPN 115.4
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