TY - JOUR
T1 - Extraction and determination of trace amounts of energetic compounds in blood by gas chromatography with electron capture detection (GC/ECD)
AU - Zhang, Baohong
AU - Pan, Xiaoping
AU - Smith, Jordan N.
AU - Anderson, Todd A.
AU - Cobb, George P.
N1 - Funding Information:
The authors would like to thank Dr. J.M. Hellman of the Animal Care and Use Committee, Texas Tech University for kindly providing pig blood samples. This work is funded by the U.S. Department of Defense contract CU1235, through the Strategic Environmental Research and Development Program (SERDP). An EPA STAR fellowship supported J.N.S.
PY - 2007/4/30
Y1 - 2007/4/30
N2 - This paper describes an efficient and sensitive method for determining five energetic compounds at trace levels (ng/mL) in blood by gas chromatography with electron capture detection (GC/ECD). For seven test concentrations (1-1250 ng/mL), the average recoveries (%) were 104 ± 16, 108 ± 22, 105 ± 14, 100 ± 22 and 108 ± 16 for hexahydro-1,3,5-trinitroso-1,3,5-triazine (TNX), hexahydro-1,3-dinitroso-5-nitro-1,3,5-triazine (DNX), hexahydro-1-nitroso-3,5-dinitro-1,3,5-triazine (MNX), hexahydro-1,3,5-trinitro-1,3,5-triazacyclohexane (RDX) and 2,4,6-trinitrotoluene (TNT) (n = 84), respectively. Analysis of DNX and RDX produced lower precision than other energetic compounds. Acetonitrile extracts of blood samples should be analyzed immediately as the test compounds can transform into unknown compounds, which lowered the recovery by 0-45% within 10 days at room temperature (∼20 °C). Maintaining sample extracts at 4 °C decreased loss of test compounds. The method described herein was validated by different analysis teams on different days. Two-way ANOVA indicated that there was no significant difference between analysis teams or days of analysis. The method was successfully employed in the analysis of blood samples from a mouse dosing study involving TNX and RDX.
AB - This paper describes an efficient and sensitive method for determining five energetic compounds at trace levels (ng/mL) in blood by gas chromatography with electron capture detection (GC/ECD). For seven test concentrations (1-1250 ng/mL), the average recoveries (%) were 104 ± 16, 108 ± 22, 105 ± 14, 100 ± 22 and 108 ± 16 for hexahydro-1,3,5-trinitroso-1,3,5-triazine (TNX), hexahydro-1,3-dinitroso-5-nitro-1,3,5-triazine (DNX), hexahydro-1-nitroso-3,5-dinitro-1,3,5-triazine (MNX), hexahydro-1,3,5-trinitro-1,3,5-triazacyclohexane (RDX) and 2,4,6-trinitrotoluene (TNT) (n = 84), respectively. Analysis of DNX and RDX produced lower precision than other energetic compounds. Acetonitrile extracts of blood samples should be analyzed immediately as the test compounds can transform into unknown compounds, which lowered the recovery by 0-45% within 10 days at room temperature (∼20 °C). Maintaining sample extracts at 4 °C decreased loss of test compounds. The method described herein was validated by different analysis teams on different days. Two-way ANOVA indicated that there was no significant difference between analysis teams or days of analysis. The method was successfully employed in the analysis of blood samples from a mouse dosing study involving TNX and RDX.
KW - Blood
KW - Electron capture detection
KW - Energetic compound
KW - Explosive
KW - Gas chromatography
UR - http://www.scopus.com/inward/record.url?scp=34047261758&partnerID=8YFLogxK
U2 - 10.1016/j.talanta.2006.11.026
DO - 10.1016/j.talanta.2006.11.026
M3 - Article
C2 - 19071663
AN - SCOPUS:34047261758
VL - 72
SP - 612
EP - 619
JO - Talanta
JF - Talanta
SN - 0039-9140
IS - 2
ER -