International comparison on the determination of polychlorinated biphenyl congeners in sediment

CCM.M-K4 is a key international comparison organized by the Bureau International des Poids et Mesures (BIPM) to verify the measurement ability of 1kg stainless weights. This paper reports the process analysis of mass determination of CCM.M-K4 during the measurement in NIM, China. The gravity correction and air bouncy correction are discussed, and the measuring uncertainties of measurement process are evaluated. Mass difference between the test standards is 0.0015 mg, and average mass of both test standards is 0.013 mg. The standard uncertainty of test weights is 0.013 mg.

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Determination of Organochlorine Pesticide and Polychlorinated Biphenyl Residues in Fatty Fish by Tandem Solid-Phase Extraction Cleanup

Journal of AOAC International ◽

10.1093/jaoac/79.5.1209 ◽

1996 ◽

Vol 79 (5) ◽

pp. 1209-1214 ◽

Cited By ~ 9

Author(s):

Frank J Schenck ◽

Lori Calderon ◽

Lynda V Podhorniak

Keyword(s):

Solid Phase Extraction ◽

Organochlorine Pesticide ◽

Pesticide Residues ◽

Polychlorinated Biphenyl ◽

Solid Phase ◽

Electron Capture Detection ◽

Phase Extraction ◽

Fatty Fish ◽

Organochlorine Pesticide Residues

Abstract A rapid, multiresidue solid-phase extraction (SPE) technique for determination of organochlorine pesticide and polychlorinated biphenyl (PCB) residues in nonfatty fish was modified for use with fatty fish. In the modified procedures, samples are extracted with acetonitrile, and the extract is cleaned up with both C18 and Florisil SPE columns. Residues are determined by gas chromatography with electron capture detection. The original method was modified for use with fatty fish by reducing the amount of tissue extracted and by using an improved Florisil SPE cleanup. Recovery data are presented for 24 fortified organochlorine pesticide residues (0.12 ppm) and 3 fortified PCB residues (0.80 ppm) from flounder, bluefish, and shad samples, which contained 0.8,5.4, and 22.6% fat, respectively. For the 3 types of fish, recoveries of 23 of 24 fortified organochlorine pesticide residues ranged from 55 to 129%, and recoveries of 3 fortified PCB residues ranged from 55 to 104%. There were no significant differences in recovery based on fish species and/or fat content for the majority of residues studied. This SPE method and the official AOAC method yielded comparable results for fish containing incurred organochlorine residues.

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Multiresidue Method for Determination of Organochlorine Insecticides and Polychlorinated Biphenyl Congeners in Fatty Processed Foods

Journal of AOAC International ◽

10.1093/jaoac/79.6.1434 ◽

1996 ◽

Vol 79 (6) ◽

pp. 1434-1446 ◽

Cited By ~ 17

Author(s):

Anna Sannino ◽

Paola Mambriani ◽

Mirella Bandini ◽

Luciana Bolzoni

Keyword(s):

Polychlorinated Biphenyl ◽

Methylene Chloride ◽

Gas Chromatography Mass Spectrometry ◽

Animal Origin ◽

Electron Capture Detection ◽

Matrix Interference ◽

Selected Ion Monitoring ◽

Pcb Congeners ◽

Organochlorine Insecticides

Abstract A previously published gel permeation chromatographic (GPC) procedure for determination of organophosphorous insecticides is used to determine 24 organochlorine (OC) pesticide and 9 polychlorinated biphenyl (PCB) residues in 8 fatty preserved foods of vegetable and animal origin. Samples are extracted with methylene chloride and cleaned up by automated GPC with a Biobeads SX3 column and a methylene chloride–cyclohexane (15 + 85) eluant. Compounds are quantitated by gas chromatography/mass spectrometry (GC/MS) with selected ion monitoring using a DB-5 column. Average recoveries of OC pesticides from samples fortified at 0.010–0.080 mg/kg ranged from 73 to 98%. Average recoveries of 9 PCB congeners spiked at 2 levels (0.0025 and 0.020 mg/kg) were between 85 and 104%. Quantitation limits were between 0.002 and 0.025 mg/kg, depending on the compound. The purified extracts were analyzed further by GC with electron capture detection (ECD), and the results were compared with those obtained by MS. Determination of some OC pesticides and PCB congeners was not possible by ECD because of matrix interference.

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