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Sample Analysis

Pesticides in Baby Food: Sample Analysis

July 1, 1995

Appendix 2

Organochlorine Pesticides

a. Chlorinated with Hall detector on HP 5890 GC.

  • Column: DB17 30m x 0.53mm ID, OI 4420 ELCD Detector
  • Temperatures: 80C (1min) to 180C @30C/min (0 Hold) to 300C @3.6C/min 7 min hold.
  • Inj. Temp: 230C
  • Inj. Vol: 3ul

b. Chlorinated with ECD detector on HP 5890 GC.

  • Columns: DB1701 30m x 0.25mm ID, ECD detector

    DB5 30 x 0.25mm ID, ECD detector

  • Temperatures: 80C(1min) to 180 @30C/min (0 hold) to 300C @3.6C/min 7 min hold.
  • Inj. Temp: 230C
  • Inj. Vol: 1ul

Organophosphate Pesticides

a. Initial Flame Photometric Detector (FPD) on HP 5890 GC

  • Column: DB17 30m x 0.53mm ID, HP FPD P filter.
  • Temperatures: 80C(1min) to 180 @30C/min (0 hold) to 300C @3.6C/min 7 min hold.
  • Inj. Temp: 230C
  • Inj. Vol: 3ul

b. Confirmations with FPD on HP 5890 GC.

  • Column: RTX225 15m x 0.53mm ID @200C isothermal.
  • Inj. Temp: 230C
  • Inj. Vol: 3ul

Organonitrogen Pesticides

a. Initial Nitrogen Phosphorous Detector (NPD) on HP 5890 GC.

  • Column: DB1701 30m x 0.25mm ID, NPD detector

    DB5 30m x 0.25mm ID, NPD detector

  • Temperatures: 80C (1min) to 180C @30C/min (0 hold) to 300C @3.6C/min 7 min hold.
  • Inj. Temp: 230C
  • Inj. Vol: 3ul

b. Confirmations, none needed

Carbamate Pesticides

All runs on Waters, High Performance Liquid Chromatography (HPLC) with post column derivitization. Injections, 10 ul.

Organosulfur (Propargite) Pesticides

All analysis on HP 5970 Selective Ion GC Mass Spectrometer.

  • Column: DB5 Mass Spec 30m x 0.25mm ID
  • Ions Monitored: 135,350 & 351
  • Temperatures: 60C to 300C
  • Inj. Vol: 1ul

Thiabendazole

a. Initial analysis on Waters HPLC

  • Column: Zorbax Phenyl column 25cm x 4.6mm ID 5um particles
  • Flow rate: 1ml/min
  • Detector: 305nm ex 355nm em flouresence detector
  • Inj Vol: 5ul

b. Confirmations

  • Column: Supelco LC18DB 7.5cm x 4.6mm ID 3um particles
  • Flow rate: 1.5ml/min
  • Detector: 305nm ex 355nm em flouresence detector
  • Inj. Vol: 5ul

Benomyl

a. Initial Analysis on Waters HPLC

  • Column: Supelco LC18DB 7.5cm x 4.6mm ID 3 um particles
  • Flow rate: 1.5 ml/min
  • Detector: 280nm ex 305nm em flouresence detector
  • Inj. Vol: 50ul

ETU

a. Initial Analysis on Bio Analytical Systems, BAS LC 4B with Electro Chemical Detector

  • Column: Shandon Hypercarb 10cm X 4.6 mm ID
  • Flow Rate: 0.5 ml/min
  • Detector: BAS LC 4B
  • Inj. Vol: 50ul
  • Volts: 0.35