METHOD ABSTRACTS108 / POST-COLUMN LC ANALYSIS OF 23 N-METHYL CARBAMATESAN EXPANDED METHOD USING WATER/ACETONITRILE OR WATER/METHANOL GRADIENTSThere are a number of carbamate pesticide compounds employed worldwide which are not included in the 10 compoundsmandated by USEPA Method 531.1 and AOAC Pro<strong>to</strong>col 29.A05.This Application Note describes methods for separating as many as 23 compounds, using a <strong>Pickering</strong> C8, 5 µm silica, columnwith either Water/Ace<strong>to</strong>nitrile or Water/Methanol gradients. Instruments, post-column derivatization and detectionpro<strong>to</strong>cols, and reagents remain unchanged, as described <strong>Pickering</strong>’s brochure, Post-column LC Systems for Environmental PesticideAnalysis (B-CA5) and User’s Manual 0101-0002.Although there are only two co-elutions in each of the solvent gradient pro<strong>to</strong>cols, the compounds were assigned <strong>to</strong> twoseparate test mixtures, A and B, in order <strong>to</strong> demonstrate the full range of separation.The differences in selectivity between the Ace<strong>to</strong>nitrile and Methanol pro<strong>to</strong>cols enable the user <strong>to</strong> employ both solventsystems as a means of conrming peak identication.The following comparison of Ace<strong>to</strong>nitrile <strong>to</strong> Methanol might be helpful in choosing which solvent system will be for usedroutinely, and which will be for conrmation:• Ace<strong>to</strong>nitrile generally exhibits higher sensitivity and baseline noise.• It also costs more and its disposal is more restricted.Eleven of the most widely occurring carbamate compounds and BDMC (internal standard) are supplied by <strong>Pickering</strong>Labora<strong>to</strong>ries in its qualitative test mixtures, Cat. No. 1700-0063. These are designated by * in the test mixture tables below.Other compounds may be purchased from suppliers of environmental standards. A few may vary considerably in homogeneityand availability.Water/Ace<strong>to</strong>nitrileWater/Methanol1 Aldicarb sulfoxide (Standak)2 Aldicarb sulfone3 Oxamyl (Vydate)4 Methomyl (Lannate)5 3-Hydroxy carbofuran6 Aldicarb (Temik)7 Propoxur (Baygon)8 Carbofuran (Furadan)9 Carbaryl (Sevin)10 Methiocarb (Mesurol)11 BDMC internal standard12 Bu<strong>to</strong>carboxim sulfoxide13 Bu<strong>to</strong>carboxim sulfone14 Ethiofencarb sulfoxide15 Ethiofencarb sulfone16 Bu<strong>to</strong>carboxim17 Ethiofencarb18 Thiofanox Sulfoxide19 Thiofanox Sulfone20 Methiocarb sulfoxide21 Methiocarb sulfone22 3-Ke<strong>to</strong>carbofuran23 Thiofanox
METHOD ABSTRACTSAnalytical Conditions: Water/Ace<strong>to</strong>nitrile Pro<strong>to</strong>colColumn: 4.0 x 250 mm, <strong>Pickering</strong> Cat.No. 0840250Sample Injection: 10 µl in MeOH (for all chroma<strong>to</strong>grams shown)Mobile Phase:Solvent A: HPLC-grade WaterSolvent B: HPLC-grade Ace<strong>to</strong>nitrile (ACN)Program:TIME H 2O % ACN % GRADIENT0 90 102 90 10 Isocratic46 49 51 Linear46.1 30 70 Step49 30 70 IsocraticEquilibration Time: 13 minutesEluant Flow Rate: 0.80 mL/minuteColumn Temperature: 37 CReagent 1: 0.3 mL/minute, CB130 Hydrolysis ReagentReagent 2: 0.3 mL/minute, OPA reagent 1 for derivatizationReac<strong>to</strong>rs:Hydrolysis: 100 C, 500 µLDerivatization: Ambient, 100 µLFl<strong>our</strong>escence Detection:Excitation: 330 nmEmission: 465 nmAnalytical Conditions: Water/Methanol Pro<strong>to</strong>colMobile Phase:Solvent A: HPLC-grade WaterSolvent B: HPLC-grade Methanol (MeOH)Program:TIME H 2O % MeOH % GRADIENT0 88 122 88 12 Isocratic42 34 66 Linear46 34 66 Isocratic46.1 0 100 Step49 0 100 Isocratic1131 o-Phthalaldehyde (O120) and Thiofl <strong>our</strong> (3700-2000), <strong>Pickering</strong>’sbrand of Dimethylaminoethanethiol•HCI, in OPA Diluent (CB910)REFERENCE:R.T. Krause, J. Chroma<strong>to</strong>graphy, 185, 615-624 (1979)R.T. J. Chroma<strong>to</strong>graphic Science, 16, 281-288 (1978)H.A. Moye, S.J. Scherer and P.A. St. John, Anal. Letters, 10, 1049-1073 (1977)A. de Kok and M. Hiemstra, J. AOAC int’l, 75, 1063-1072 (1992)Offi cial Methods of Analysis, 15th Ed., AOAC Int’l, Arling<strong>to</strong>n, VA, (291-293)Method 531.1, U.S. Environmental Protection AgencyPRODUCT CATALOGPICKERING LABORATORIES10/11
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TABLE OF CONTENTSINTRODUCTION3 Cust
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INTRODUCTIONINSTALLATION & TRAINING
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“A LOT HAS CHANGED SINCE PRODUCIN
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INSTRUMENTS & HARDWAREFEATURE HIGHL
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INSTRUMENTS & HARDWARE• Indoor us
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ELUANTSCHROMATOGRAPHIC GRADEPickeri
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APPLICATION KITSAmino Acid Analysis
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