Page:NIOSH Manual of Analytical Methods - 5007.pdf/1

 ROTENONE

C23 H22 O6

MW: 394.43

CAS: 83-79-4

METHOD: 5007, Issue 2

5007

RTECS: DJ2800000

EVALUATION: FULL

OSHA : 5 mg/m 3 NIOSH: 5 mg/m 3; Group II Pesticide ACGIH: 5 mg/m 3

PROPERTIES:

Issue 1: 15 February 1984 Issue 2: 15 August 1994

solid, MP 163 °C or 181 °C; BP 220 °C @ 0.5 mm Hg; d ca. 1 g/cm 3; VP not significant

SYNONYMS: tubatoxin; cube

SAMPLING SAMPLER:

FILTER (1-mm PTFE membrane)

FLOW RATE:

1 to 4 L/min

VOL-MIN: -MAX:

8L 400 L

SHIPMENT:

routine

SAMPLE STABILITY:

MEASUREMENT

at least 7 days @ 25 °C in dark

BLANKS:

2 to 10 field blanks per set

BULK SAMPLE:

desirable; 1 g

ACCURACY 3

RANGE STUDIED:

1 to 11 mg/m [1] (100-L sample)

BIAS:

- 0.6%

ˆ ): OVERALL PRECISION (S rT

0.079

ACCURACY:

± 13.5%

TECHNIQUE:

HPLC; UV DETECTION

ANALYTE:

Rotenone

EXTRACTION:

4 mL acetonitrile; 30 min

INJECTION VOLUME:

10 µL

MOBILE PHASE:

60% methanol/40% water, 2 mL/min

DETECTOR:

UV @ 290 nm; 0.1A full-scale; 1-cm cell

COLUMN:

µ-Bondapak C 18 (30 cm x 3.9-mm ID stainless steel); ambient temperature

CALIBRATION:

solutions of Rotenone in acetonitrile

RANGE:

0.04 to 1 mg per sample

ESTIMATED LOD:

4 µg per sample [1,2]

PRECISION (Sr):

0.024 [1]

APPLICABILITY: The working range is 0.4 to 10 mg/m 3 for a 100-L air sample and the method is applicable to commercial formulations.

INTERFERENCES: None known. Rotenone, a naturally occurring insecticide, is adequately separated by HPLC from other compounds (e.g., sumatrol, α-toxicarol, deguelin, elliptone, malaccol, and tephrosin [3]) present in commercial cube root extracts [4]. Rotenone is sensitive to photodecomposition.

OTHER METHODS: This is Method S300 [2] in a revised format.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94