Sulfonylurea herbicides are a group of non-selective herbicides that act by disrupting plant protein synthesis. They have been introduced relatively recently and are widely used, but application rates are relatively low. Potential sources for human exposure include foods grown in treated soil or contaminated water. Urinary measurement of sulfonylurea herbicides can be used to assess human exposure.
Bensulfuron methyl (URXBSM), Chlorsulfuron (URXCHS), Ethametsulfuron methyl (URXEMM), Foramsulfuron (URXFRM), Halosulfuron (URXHLS), Mesosulfuron methyl (URXMSM), Metsulfuron methyl (URXMTM), Nicosulfuron (URXNOS), Oxasulfuron (URXOXS), Primisulfuron methyl (URXPIM), Prosulfuron (URXPRO), Rimsulfuron (URXRIM), Sulfometuron methyl (URXSMM), Sulfosulfuron (URXSSF), Thifensulfuron methyl (URXTHF), Triasulfuron (URXTRA), Triflusulfuron-methyl (URXTRN)
Because of their increasing use in agricultural applications, a method to measure both occupational and incidental human exposures to Sulfonylurea herbicides was developed.
Participants aged 6 years and older who met the subsample requirements.
Bensulfuron methyl (URXBSM), Chlorsulfuron (URXCHS), Ethametsulfuron methyl (URXEMM), Foramsulfuron (URXFRM), Halosulfuron (URXHLS), Mesosulfuron methyl (URXMSM), Metsulfuron methyl (URXMTM), Nicosulfuron (URXNOS), Oxasulfuron (URXOXS), Primisulfuron methyl (URXPIM), Prosulfuron (URXPRO), Rimsulfuron (URXRIM), Sulfometuron methyl (URXSMM), Sulfosulfuron (URXSSF), Thifensulfuron methyl (URXTHF), Triasulfuron (URXTRA), Triflusulfuron-methyl (URXTRN)
A method for measuring 17 sulfonylurea (SU) herbicides in human urine was developed. Urine samples were extracted using solid phase extraction (SPE), pre-concentrated, and analyzed by high-performance liquid chromatography–tandem mass spectrometry using turbo-ionspray atmospheric pressure ionization. Carbon 13-labeled ethametsulfuron methyl was used as an internal standard. Chromatographic retention times were under 7 minutes. Total throughput was estimated as >100 samples per day. The limits of detection (LOD) ranged from 0.05 µg/L to 0.10 µg/L with an average LOD of 0.06 µg/L. Average total relative standard deviations were 17%, 12% and 8% at 0.1 µg/L, 3.0 µg/L and 10 µg/L, respectively. Average extraction efficiencies of the SPE cartridges were 87% and 86% at 2.5 µg/L and 25 µg/L, respectively. Chemical degradation in acetonitrile and urine was monitored over 250 days. Estimated days for 10% and 50% degradation in urine and acetonitrile ranged from 0.7 days to >318 days.
Urine specimens are processed, stored, and shipped to the Division of 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.
Analytical Laboratories
NHANES uses several methods to monitor the quality of the analyses performed by the 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.
NCEH developed and distributed a quality control protocol for all the laboratories which outlined the Westgard rules used when running NHANES specimens. Any problems encountered during shipping or receipt of specimens, instrument calibration, reagents, and any special considerations are submitted to NCHS and Westat. Summary statistics for each control pool, QC graphs, are reviewed by NCHS 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 Sciences’ quality control and quality assurance performance criteria for accuracy and precision (similar to specifications outlined by Westgard (1981).
Subsample weights
Measures of urinary current use pesticide metabolites were measured in a one third subsample of persons 6 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.
Variance estimation
The analysis of NHANES laboratory data must be conducted with the key survey design and basic demographic variables. The NHANES 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.
Detection Limits
Two variables are provided for each of these analytes. The variable named URD___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 URX___ provides the analytic result for that analyte.
The detection limit divided by the square root of 2 is the value that is provided for results that are below the limit of detection.
Please refer to the Analytic Guidelines for further details on the use of sample weights and other analytic issues.
Angerer, J.; Ritter, A. J. Chromatogr., B 1997, 695, 217-226.
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.Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 to 475173.70936 | Range of Values | 2756 | 2756 | |
. | Missing | 0 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0354 to 0.0354 | Range of Values | 2634 | 2634 | |
. | Missing | 122 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2634 | 2634 | |
. | Missing | 122 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0354 to 0.0354 | Range of Values | 2419 | 2419 | |
. | Missing | 337 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2419 | 2419 | |
. | Missing | 337 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0707 to 0.33 | Range of Values | 2634 | 2634 | |
. | Missing | 122 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 6 | 6 | |
1 | Below lower detection limit | 2628 | 2634 | |
. | Missing | 122 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0424 to 0.0424 | Range of Values | 2534 | 2534 | |
. | Missing | 222 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2534 | 2534 | |
. | Missing | 222 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0495 to 0.0495 | Range of Values | 2485 | 2485 | |
. | Missing | 271 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2485 | 2485 | |
. | Missing | 271 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0354 to 0.0354 | Range of Values | 2634 | 2634 | |
. | Missing | 122 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2634 | 2634 | |
. | Missing | 122 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0354 to 0.0354 | Range of Values | 2634 | 2634 | |
. | Missing | 122 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2634 | 2634 | |
. | Missing | 122 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0707 to 0.0707 | Range of Values | 2570 | 2570 | |
. | Missing | 186 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2570 | 2570 | |
. | Missing | 186 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0424 to 0.0424 | Range of Values | 2634 | 2634 | |
. | Missing | 122 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2634 | 2634 | |
. | Missing | 122 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0424 to 0.0424 | Range of Values | 2455 | 2455 | |
. | Missing | 301 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2455 | 2455 | |
. | Missing | 301 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0354 to 0.0354 | Range of Values | 2461 | 2461 | |
. | Missing | 295 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2461 | 2461 | |
. | Missing | 295 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0424 to 0.0424 | Range of Values | 2593 | 2593 | |
. | Missing | 163 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2593 | 2593 | |
. | Missing | 163 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0354 to 0.0354 | Range of Values | 2598 | 2598 | |
. | Missing | 158 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2598 | 2598 | |
. | Missing | 158 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0354 | 0.0354 | 2593 | 2593 | |
. | Missing | 163 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2593 | 2593 | |
. | Missing | 163 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0566 to 0.0566 | Range of Values | 2634 | 2634 | |
. | Missing | 122 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2634 | 2634 | |
. | Missing | 122 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0495 to 0.0495 | Range of Values | 2557 | 2557 | |
. | Missing | 199 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2557 | 2557 | |
. | Missing | 199 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0.0354 to 0.0354 | Range of Values | 2562 | 2562 | |
. | Missing | 194 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
0 | At or above the detection limit | 0 | 0 | |
1 | Below lower detection limit | 2562 | 2562 | |
. | Missing | 194 | 2756 |
Code or Value | Value Description | Count | Cumulative | Skip to Item |
---|---|---|---|---|
7 to 678 | Range of Values | 2671 | 2671 | |
. | Missing | 85 | 2756 |