Organic fluorochemicals are used in multiple commercial applications including surfactants, lubricants, paints, polishes, food packaging and fire-retarding foams. Several of these polyfluorochemicals (PFCs) are ubiquitous contaminants found both in humans and animals worldwide. Perfluorooctane sulfonate (PFOS) has been used in a wide variety of industrial and consumer products including protective coatings for carpets and apparel, paper coatings, insecticide formulations, and surfactants. In May 2000, the 3M Company, the sole manufacturer of PFOS in the United States and the principal manufacturer worldwide, announced that it was discontinuing the production of perfluorooctanyl fluoride-based chemistries, including PFOS. Perfluorooctanoic acid (PFOA) is used primarily to produce its salts which are used in the production of fluoroelastomers and fluoropolymers, such as polytetrafluoroethylene (PTFE) and polyvinylidine fluoride (PVDF). PTFE has numerous uses in many industrial and consumer products, including coatings on textiles and carpet; uses in the automotive, mechanical, aerospace, chemical, electrical, medical, and building/construction industries; personal care products; and non-stick coatings on cookware. PVDF is used primarily in electrical/electronics, building/construction, and chemical processing industrial sectors.
Participants aged 12 years and older who met the subsample requirements.
Description of Laboratory Methodology
The test principle utilizes solid phase extraction-high performance liquid chromatography-turboionspray ionization-tandem mass spectrometry (SPE-HPLC-TCI-MS/MS) for the quantitative detection of PFCs: perfluorooctane sulfonamide (PFOSA), 2-(N-methyl-perfluorooctane sulfonamido) acetic acid (Me-PFOSA-AcOH), 2-(N-ethyl-perfluorooctane sulfonamido) acetic acid (Et-PFOSA-AcOH), perfluorohexane sulfonate (PFHxS), PFOS, perfluoropentanoate (PFPeA), perfluorohexanoate (PFHxA), perfluoroheptanoate (PFHpA), PFOA, perfluorononanoate (PFNA), perfluorodecanoate (PFDeA), perfluoroundecanoate (PFUA), and perfluorododecanoate (PFDoA) (16). The PFCs are extracted from serum using an automated SPE procedure, separated from other extracted components in the SPE eluate by reversed phase HPLC, and detected by negative ion TIS-MS/MS using a multiple reaction monitoring experiment. This method allows for rapid detection of these fluorochemicals in human serum with limits of detection in the low parts per billion (ppb or ng/mL) range.
Laboratory Quality Assurance and Monitoring
Serum specimens are processed, stored, and shipped to the Division of Environmental Health Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention for analysis.
Detailed specimen collection and processing instructions are discussed in the NHANES Laboratory/Medical Technologists Procedures Manual (LPM). Vials are stored under appropriate frozen (–20°C) conditions until they are shipped to National Center for Environmental Health for testing.
Mobile Examination Centers (MECs)
Laboratory team performance is monitored using several techniques. NCHS and contract consultants use a structured quality assurance evaluation during unscheduled visits to evaluate both the quality of the laboratory work and the quality-control procedures. Each laboratory staff person is observed for equipment operation, specimen collection and preparation; testing procedures and constructive feedback are given to each staff. Formal retraining sessions are conducted annually to ensure that required skill levels were maintained.
The NHANES QA/QC protocols meet the 1988 Clinical Laboratory Improvement Act mandates. Detailed QA/QC instructions are discussed in the NHANES LPM.
NHANES uses several methods to monitor the quality of the analyses performed by the contract laboratories. In the MEC, these methods include performing blind split samples collected on “dry run” sessions. In addition, contract laboratories randomly perform repeat testing on 2.0% of all specimens.
NCHS developed and distributed a quality control protocol for all the contract laboratories which outlined the Westgard rules used when running NHANES specimens. Progress reports containing any problems encountered during shipping or receipt of specimens, summary statistics for each control pool, QC graphs, instrument calibration, reagents, and any special considerations are submitted to NCHS and Westat quarterly. The reports are reviewed for trends or shifts in the data. The laboratories are required to explain any identified areas of concern.
All QC procedures recommended by the manufacturers were followed. Reported results for all assays meet the Division of Laboratory Science’s quality control and quality assurance performance criteria for accuracy and precision (similar to specifications outlined by Westgard (1981).
Measures of serum polyfluorinated chemicals were measured in a one third subsample of persons 12 years and over. Special sample weights are required to analyze these data properly. Specific sample weights for this subsample are included in this data file and should be used when analyzing these data.
The analysis of NHANES 2003-2004 laboratory data must be conducted with the key survey design and basic demographic variables. The NHANES 2003-2004 Demographic Data File contains demographic and sample design variables. The recommended procedure for variance estimation requires use of stratum and PSU variables (SDMVSTRA and SDMVPSU, respectively) in the demographic data file.
Links to NHANES Data Files
This laboratory data file can be linked to the other NHANES 2003-2004 data files using the unique survey participant identifier SEQN.
The detection limits were constant for all of the analytes in the data set. Two variables are provided for each of these analytes. The variable named LBD___LC indicates whether the result was below the limit of detection. There are two values: “0” and “1”. “0” means that the result was at or above the limit of detection. “1” indicates that the result was below the limit of detection.
The other variable named LBX___ provides the analytic result for that analyte.
The constant lower limits of detection for each polyfluorochemical is:
Constant Lower Limits of Detection for Polyfluorochemicals
| Perfluorooctanoic acid
| Perfluorooctane sulfonic acid
| Perfluorohexane sulfonic acid
| 2-(N-Ethyl-perfluorooctane sulfonamido) acetic acid
| 2-(N-Methyl-perfluorooctane sulfonamido) acetic acid
| Pefluorodecanoic acid
| Perfluorobutane sulfonic acid
| Perfluoroheptanoic acid
| Perfluorononanoic acid
| Perfluorooctane sulfonamide
| Perfluoroundecanoic acid
| Perflurododecanoic acid
Please refer to the Analytic Guidelines for further details on the use of sample weights and other analytic issues.