PMID- 22649943
OWN - NLM
STAT- MEDLINE
DCOM- 20120730
LR  - 20191112
IS  - 1060-3271 (Print)
IS  - 1060-3271 (Linking)
VI  - 95
IP  - 2
DP  - 2012 Mar-Apr
TI  - Evaluation of headspace solid-phase microextraction for analysis of phosphine 
      residues in wheat.
PG  - 549-53
AB  - In headspace (HS) analysis, a fumigant is released from a commodity into a 
      gas-tight container by grinding, heating, or microwaves. A new technique uses 
      HS-solid-phase microextraction (SPME) for additional preconcentration of 
      fumigant. HS-SPME was tested for detection of phosphine (PH3), chosen for 
      examination because of its wide use on stored commodities. PH3 was applied to 50 
      g wheat in separate 250 mL sealed flasks, which were equipped either with a 
      septum for conventional HS analysis or with one of four HS-SPME fibers [100 
      microm polydimethylsiloxane (PDMS), 85 microm carboxen (CAR)/PDMS, 75 microm 
      CAR/PDMS, and 65 pm PDMS/divinylbenzene (DVB)]. The wheat was heated at 45 
      degrees C for 20 min. In conventional HS analysis, a gaseous aliquot (80 pL) was 
      taken from the HS and injected into the GC instrument. In the HS-SPME procedure, 
      the fiber was removed from the HS and exposed in the heated injection port of the 
      GC instrument. In all cases, PH3 was determined under the same chromatographic 
      conditions with a GC pulsed flame photometric detector. In a comparison of the 
      efficacy of the fibers, the bipolar fibers (CAR/PDMS and PDMS/DVB) contained more 
      PH3 than the aliquot in the conventional HS analysis; larger size bipolar fibers 
      extracted PH3 more efficiently than smaller fibers (e.g., 85 > 75 > 65 microm). 
      The nonpolar fiber (PDMS) contained no PH3. Four fortification levels of PH3 on 
      wheat were tested: 0.01, 0.05, 0.1, and 0.3 microg/g. The response of each 
      bipolar fiber increased with the fortification levels, but the conventional HS 
      analysis detected no fumigant at the lowest fortification level of 0.01 mg/g. 
      Under the conditions of the validation study, the LOD was in the range of 
      0.005-0.01 ng PH3/g wheat.
FAU - Ren, Yong Lin
AU  - Ren YL
AD  - Cooperative Research Centre for National Plant Biosecurity, Canberra, Australia. 
      y.ren@murdoch.edu.au
FAU - Padovan, Benjamin
AU  - Padovan B
FAU - Desmarchelier, James M
AU  - Desmarchelier JM
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
PL  - England
TA  - J AOAC Int
JT  - Journal of AOAC International
JID - 9215446
RN  - 0 (Insecticides)
RN  - 0 (Pesticide Residues)
RN  - 0 (Phosphines)
RN  - FW6947296I (phosphine)
SB  - IM
MH  - Food Analysis/methods
MH  - Insecticides/*chemistry
MH  - Pesticide Residues/*chemistry
MH  - Phosphines/*chemistry
MH  - Sensitivity and Specificity
MH  - Solid Phase Microextraction/*methods
MH  - Triticum/*chemistry
EDAT- 2012/06/02 06:00
MHDA- 2012/07/31 06:00
CRDT- 2012/06/02 06:00
PHST- 2012/06/02 06:00 [entrez]
PHST- 2012/06/02 06:00 [pubmed]
PHST- 2012/07/31 06:00 [medline]
AID - 10.5740/jaoacint.10-514 [doi]
PST - ppublish
SO  - J AOAC Int. 2012 Mar-Apr;95(2):549-53. doi: 10.5740/jaoacint.10-514.