Presep® Agri Series

SPE Column for Pesticides Analysis

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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)

  • 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)

  • 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)
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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)

  • 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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SPE Column

HPLC Column

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Author: Y. Higai

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