3-BROMOPROPIONIC ACID in URINE
8324
metabolite of 1-bromopropane
FORMULA: C3H5BrO2 METHOD: 8324, Issue 1
MW: 152.97 CAS: 590-92-1 EVALUATION: FULL
Published limits and guidelines using this compound as a marker: OSHA: None NIOSH: None Other OELs: [1,2,3,4]*
BIOLOGICAL INDICATOR OF:
RTECS: UE7875000 Issue 1: 29 August 2014
Exposure to 1-bromopropane
PROPERTIES: Solid; d 1.48 g/mL at 25 oC; MP 58-62 oC
SYNONYMS: β-Bromopropionic acid; 2-carboxyethylbromide. SAMPLING SPECIMEN: Urine VOLUME:
MEASUREMENT TECHNIQUE:
GAS CHROMATOGRAPHY, MASS SPECTROMETRY with SELECTED ION MONITORING (GC/MS-SIM)
ANALYTE:
tert-butyldimethylsilane derivative of 3-bromopropionic acid
EXTRACTION:
Liquid-liquid extraction (LLE)
INJECTION VOLUME:
0.5 μL, splitless
At least 15 mL
PRESERVATIVE:
None added. Refrigerate or freeze upon collection.
SHIPMENT: Ship cold or frozen with ice or dry ice. Freeze upon receipt at the laboratory. SAMPLE STABILITY: Stable in frozen urine for at least 30 days. CONTROLS: Urine specimens obtained from non-exposed individuals. ACCURACY
TEMPERATURES INJECTION: 200 oC COLUMN:
60 oC initial, 4 oC/min to 180 oC,15 oC/min to 255 oC, post-run at 270 oC for 5 min
DETECTOR:
Source 230 oC, Quadrupole 150 oC; Solvent delay, 15 min
RANGE STUDIED:
RUN TIME:
Approximately 50 minute cycle time
Table 1
CARRIER GAS:
Helium, 0.8 mL/min constant flow
BIAS:
None established
COLUMN:
Capillary, fused silica, 100% dimethylpolysiloxane, 50 m X 0.20 mm (ID), 0.33 μm film thickness
CALIBRATION:
Analyte in control urine; with internal standard
PRECISION: Table 1 RECOVERY ACCURACY: Full recovery (95% overall) was established by a spiked urine recovery, overall RSD was +3.1% (Table 1). The definitions of precision and accuracy in this method are those utilized by the US Food and Drug Administration [5].
QUALITY CONTROL:
RANGE:
At least one level of spiked urine sample prepared from a separately weighed stock solution 2.0 to 100 μg/mL
ESTIMATED LOD: Approximately 0.01 μg/mL (IUPAC) [6]. 0.1 μg/mL is the lowest calibration standard. APPLICABILITY: 3-Bromopropionic acid (3-BPA) has been reported to be a rat metabolite [7] and is a potential human biomarker for exposure to 1-bromopropane. This method measures the quantity of free 3-BPA in urine. 1-Bromopropane is used as an industrial solvent. In one limited study, 3-BPA was not detected in individuals exposed to low levels of 1-bromopropane [8]. INTERFERENCES: None found or identified. OTHER METHODS: This method is from the one described by B’Hymer and Cheever [9] and further investigated by Mathias, et al. [8].
NIOSH Manual of Analytical Methods (NMAM), Fifth Edition
