PMID- 12723927 OWN - NLM STAT- MEDLINE DCOM- 20030714 LR - 20191210 IS - 1060-3271 (Print) IS - 1060-3271 (Linking) VI - 86 IP - 2 DP - 2003 Mar-Apr TI - Comparative tests to improve the gas chromatographic analysis of chlorobornanes in fish samples. PG - 432-8 AB - A comparison was made between electron capture negative ionization quadrupole mass spectrometry (ECNI-MS) and electron capture detection (ECD) with regard to repeatability and reproducibility for the gas chromatographic (GC) analysis of toxaphene congeners [chlorobornanes (CHBs)]. The tests, including standard solutions and several cleaned fish extracts, showed larger relative standard deviations (RSDs) for the repeatability of ECNI-MS but no differences in the reproducibility of the 2 techniques. The sensitivity of the GC-ECNI-MS was considerably better than that of GC/ECD. Four stepwise-designed comparative tests were also conducted on GC analysis, cleanup, and the complete method. The results showed that, according to the current state-of-the-art, coefficients of variation for the between-laboratory performance were not < 20% and were usually between 20 and 30%. In spite of separation problems, e.g., for CHB 26, which cannot be separated into a single-component peak, a 95% methyl 5% phenyl polysiloxane (CP Sil 8) column was preferred to more polar columns for the analysis of CHBs 26, 40, 41, 44, 50, and 62. CHB 62 was more difficult to determine than CHB 26 and 50. Addition of the CHBs 40, 41, and 44 to the standard set of 3 chlorobornanes (26, 50, and 62) resulted in more separation problems. A 3-step cleanup method was recommended. FAU - de Boer, Jacob AU - de Boer J AD - Netherlands Institute for Fisheries Research, PO Box 68, 1970 AB IJmuiden, The Netherlands. j.deboer@rivo.wag-ur.nl FAU - Leonards, Pim E G AU - Leonards PE FAU - Klungsoyr, Jarle AU - Klungsoyr J FAU - McHugh, Brendan AU - McHugh B FAU - Nixon, Eugene AU - Nixon E FAU - McGovern, Evin AU - McGovern E FAU - Rimkus, Gerhard G AU - Rimkus GG LA - eng PT - Comparative Study 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 (Camphanes) RN - 0 (Fish Oils) RN - 0 (Insecticides) RN - 0 (Pesticide Residues) RN - 8001-35-2 (Toxaphene) SB - IM MH - Animals MH - Camphanes/*analysis MH - Chromatography, Gas MH - Electrochemistry MH - Fish Oils/analysis MH - Fishes/*metabolism MH - Insecticides/*analysis MH - Mass Spectrometry MH - Pesticide Residues/*analysis MH - Reference Standards MH - Reproducibility of Results MH - Toxaphene/*analysis EDAT- 2003/05/02 05:00 MHDA- 2003/07/15 05:00 CRDT- 2003/05/02 05:00 PHST- 2003/05/02 05:00 [pubmed] PHST- 2003/07/15 05:00 [medline] PHST- 2003/05/02 05:00 [entrez] PST - ppublish SO - J AOAC Int. 2003 Mar-Apr;86(2):432-8.