Gas Chromatographic Measurement and Identification of Pesticide Residues with Electron Capture, Microcoulometric, and Electrical Conductivity Detectors

Author(s):  
WILLIAM E. WESTLAKE
1994 ◽  
Vol 57 (5) ◽  
pp. 441-444 ◽  
Author(s):  
ANTONIO HERRERA ◽  
AGUSTIN A. ARIÑO ◽  
MARIA P. CONCHELLO ◽  
REGINA LAZARO ◽  
SUSANA BAYARRI ◽  
...  

The level of organochlorine pesticides in 229 samples of Spanish meat and meat products of different species (lamb, pork, beef and poultry) was investigated. Chlorinated residues were quantitated by gas-liquid chromatography with electron capture detector using packed and capillary columns. Hexachlorobenzene (HCB) and hexachlorocyclohexane (HCH) were detected in all samples. In general, lamb appeared to be more heavily contaminated by HCB and HCH, which reached maximums of 178 ppb (μg/kg on a fat basis) and 505 ppb, respectively. The level of HCB averaged 49 ppb in lamb; varied between 8–18 ppb in pork and beef products; and amounted to 26 ppb in fresh poultry sausages. Of the three isomers of HCH determined, the γ-HCH (lindane) was most frequently detected; 100% in lamb and pork (both meat, cured sausage and pork bologna), and 64 to 94% in fresh sausages of poultry and beef. The level of the HCH group averaged 112 ppb in lamb, 85 ppb in poultry, nearly half that much in pork and pork products, and around 20–40 ppb in beef products. Dieldrin was the only chlorocyclodiene detected: 8 to 15% in pork products, and 28% in fresh poultry sausage. The DDTs in lamb showed 83% of detection, especially in the pp' form of DDE and DDT. The overall contamination with DDT and its metabolites was found to be very moderate averaging 25 ppb, with a maximum of 91 ppb. No residues of aldrin, endrin, heptachlor, heptachlor epoxide, chlordane, methoxychlor, endosulfan or trans-nonachlor were detected.


1963 ◽  
Vol 46 (2) ◽  
pp. 209-215
Author(s):  
J Lloyd Henderson

Abstract Of the techniques available for specific pesticide residues, fly bioassay is non-specific and not very sensitive; total organic chloride determination also lacks specificity; the AOAC colorimetric method produces variable results, lacks sensitivity for low levels of residues, and does not cover the range of residues likely to be present in milk. Chromatographic tests are most satisfactory. Microcoulometric gas chromatography has many advantages but requires a skilled analyst. Electron-capture gas chromatography is promising but has not been fully developed. The Mills test, which combines column cleanup with identification by paper chromatography, is a rapid, practical screening test. In a collaborative comparison of the chromatographic procedures, microcoulometry tended to give higher results than the Mills test; electron-capture gave lower results than the other two methods. Details of all tests must be followed closely for good results.


1966 ◽  
Vol 49 (4) ◽  
pp. 768-772
Author(s):  
J G Saha

Abstract Electron capture gas chromatography has been used to measure the efficiency of an extraction and cleanup procedure for chlorinated pesticide residues in wheat. Soxhlet extraction of ground wheat with acetonitrile, followed by partition into petroleum ether and cleanup on a magnesia-Celite column has been found adequate for the determination of heptachlor, aldrin, dieldrin, and endrin in concentrations as low as 5 ppb. Recoveries of aldrin, dieldrin, and endrin ranged from 98 to 104%, while those of heptachlor were 84–92%.


1973 ◽  
Vol 56 (6) ◽  
pp. 1503-1505 ◽  
Author(s):  
Lauren G Johnson

Abstract A procedure is described for the preparation and electron capture GLC determination of pentafluorobenzyl ester and ether derivatives of 2,4-D, p,p′-DDA, 1-naphthol, p-nitrophenol, and sec.-amyl phenols. A column cleanup procedure quantitatively isolates the derivatives from excess reagents and other interferences. The method can be used as an aid in the confirmation of the identity of pesticide residues and for the quantitative determination of extracted residues.


1969 ◽  
Vol 52 (4) ◽  
pp. 790-797
Author(s):  
Bernadette Malone ◽  
Jerry A Burke

Abstract A collaborative study was made of the sweep co-distillation cleanup method for multiple residues of chlorinated pesticides in edible fats and oils with determination by electron capture GLC using a column of 15% QF-1/10% DC-200 on 80–100 Gas Chrom Q. Heptachlor epoxide, p,p’-DDE, dieldrin, p,p’-TDE, and p,p’-DDT were added at two levels to butterfat and soybean oil. Mean recoveries of pesticides ranged from 86.0 to 102.1% in soybean oil and 86.4 to 98.8% in butter.


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