【求助】POPs检测方法标准

纺织品的毒杀芬残留量测定
毒杀芬的种类很多，做比较麻烦。国内的检测方法较少，楼主您可以找找国外的方法。

The determination of toxaphene in environmental samples by negative ion electron capture high resolution mass spectrometry
Brian Fowler
Chemosphere
Volume 41, Issue 4, August 2000, Pages 487-492
Abstract:
A method is described for the analysis of toxaphene in environmental samples by high resolution gas chromatography high resolution mass spectrometry in selected ion electron capture negative ion mode. Toxaphene is detected by monitoring [M–Cl]−fragments ions of chlorobornanes (Cl6–Cl10) and chlorobornenes (Cl6–Cl7) using formal ion ratio criteria. The method shows high sensitivity and excellent specificity for the detection of chlorobornanes with negligible interference from of a wide range of common environmental organochlorines including chlordanes, PCBs and PCB-oxygen adducts. The analytical scheme is applicable to sediment and biological tissue samples and typically provide sample detection limits of less than 0.2 ng/g technical toxaphene for a 10 g sample.

Determination of toxaphene in biological samples using high resolution gc coupled with ion trap MS/MS
Hing Man Chan, Jiping Zhub and Faustinus Yeboah
Chemosphere
Volume 36, Issue 9, April 1998, Pages 2135-2148
Abstract
Toxaphene remains as a pollutant of global concern because of its persistence in the environment. Its complex combination of congeners and the lack of individual standards makes accurate measurement of toxaphene residues in environmental samples a challenge. We have developed a novel method to measure toxaphene in environmental samples using ion trap MS/MS. Adequate sensitivity for analysis of biological samples such as fish and marine mammal blubbers were achieved (around 0.02 ppb to 0.06 ppb for individual congeners and 5.6 ppb for toxaphene mixtures). Accuracy was demonstrated by good recoveries of spiked toxaphene in corn oil samples (102% for toxaphene congeners at 4 ppb and 96% for toxaphene mixture at 139 ppb level). Results of analysis of toxaphene in cod liver oil (NIST SRM 1588) using the MS/MS method compared favorably with the median round robin interlaboratory data. The major advantage of the ion trap MS/MS over the existing methods; electron capture negative ionization mass spectrometer or electron capture detector, is its excellent selectivity. Interference from other organochlorines can virtually be eliminated. Therefore, the developed MS/MS method can be used as a reliable alternative to high resolution mass spectrometer for measurement of toxaphene in environmental samples with relatively low cost instrumentation.

这两篇是SD数据库中的，如果需要可以去文献求助应助版求全文。

Determination of toxaphene in soil by electron-capture negative-ion mass spectrometry and capillary column gas chromatography
ONUSKA F. I. ; TERRY K. A. ; SEECH A. ; ANTONIC M. ;
Journal of chromatography ISSN 0021-9673 CODEN JOCRAM
1994, vol. 665, no 1 (9 ref.), pp. 125-132
Abstract:
Although toxaphene is now limited in use, interest in its analysis continues because of its persistence and widespread atmospheric transport in the environment and its presence in many dump-sites all over the world. Top soil samples collected from a dump site were analyzed for toxaphene residues. Analyses were performed by wall-coated open tubular column gas chromatography in tandem with electron-capture negative-ion mass spectrometry. Since the concentrations of toxaphene residues were at mg/kg levels, the application of a mass spectrometer as a substance-selective detector has been applied.

Determination of Toxaphene in Fish From Northern Europe
van der Valk, F | Wester, PG
Chemosphere CMSHAF, Vol. 22, No. 1/2, p 57-66, 1991.
Abstract:
Concentrations of toxaphene were determined in fish from The Netherlands and adjacent marine areas by gas chromatography/negative chemical ionization-mass spectrometry, after a thorough clean-up. Levels of toxaphene lay between 0.1 and 7 mg/kg on a lipid basis. In general the measured levels were quite low, with the exception of herring oil from the Baltic Sea. In the Dutch great rivers, uniform concentrations of 0.3 mg/kg lipid in eel were found, despite the non-existence of polychlorinated terpene (PCT) use in their respective watersheds. Atmospheric transport was determined to be the most plausible cause. A major problem with the technique was the complexity of the mixture to be analyzed; this lead to an incomplete separation of the components. Toxaphene components showing different environmental behavior were distinguished, and indicated that the pattern of PCT congeners varied markedly among and between the samples and the toxaphene standard. This variety of congener patterns in different fish species suggest that the degradation capability of the fish determines the quality of PCT components which persist in the tissue. (VerNooy-PTT)

Determination of toxaphene in human milk from Nicaragua and in fish and marine mammals from the northeastern Atlantic and the North Sea
DE BOER J. ; WESTER P. G. ;
Chemosphere
1993, vol. 27, no 10 (27 ref.), pp. 1879-1890
Abstract:
Concentrations of toxaphene (polychlorinated monoterpenes, chlorobornanes) were determined in human milk samples from Nicaragua and in fish from the North Sea. Relatively high toxaphene levels were found in the Nicaraguan human milk samples. The lack of correlation between the number of children of the mothers and toxaphene levels in their milk suggests a compensation of the elimination of toxaphene by a regularly high toxaphene intake. The increasing trend of toxaphene concenatrations in North Sea fish sampled further away from the European coast suggests an aerial transport of toxaphene from the American continent to Europe

楼主还可以参考EPA525.2方法，是固相萃取水中的多种污染物的，其中包括了毒杀芬。

相关的ADI值可以参考： http://www.instrument.com.cn/bbs/shtml/20090128/1713584/