... treatment of angina pectoris many years ago
[2]; the pharmacological e ect of the dilation of the coronary arteries was found due to the
action of nitrogen monoxide produced by decomposition of alkyl ... ingestion of 10–15 mL of each alkyl nitrite causes serious methe-
moglobinemia [6]. e LD
50
value for an alkyl nitrite is reported to be 205 mg/kg. ere are not
many cases ofanalysisof alkyl ... eld of forensic toxicology. In this chapter, the
methods for analysisof the compounds by headspace (HS)-gas chromatography (GC) and
liquid-liquid extraction-GC are presented.
Determination of...
... Paasivirta J et al. (1981) Trace Analysisof Chemical Warfare Agents. An Approach to the
Environmental Monitoring of Nerve Agents. Ministry of Foreign Affairs of Finland, Helsinki, pp 27, 28, ... metabolites of VX, could
be detected [18].
GC/MS analysis for EMPA in serum. (a) a TIC and mass chromatograms; (b) an EI mass spectrum of
the t-BDMS derivative of EMPA; (c) a CI mass spectrum of the ... stream of nitrogen gas at room temperature
e
.
iii. e residue is dissolved in 100 µL of the dichloromethane solution of DAEMO (IS solu-
tion); a 1-µL of it is injected into GC/MS for analysis...
... GC/MS analysisof ∆
9
-THC-11-oic acid in human urine
[15, 16].
e) A method of silylation of glassware to be done before analysis was reported [17]; such treat-
ment suppresses the adsorption of ... 10:316–323
14) Yamamoto I (1992) Methods for analysisof cannabis and its components. In: The Pharmaceutical Society of
Japan (ed) Standard Methods of Chemical Analysis in Poisoning – With Commentaries, ... spectra of ∆
9
-THC-11-oic acid a er the TMS and methyl ester-TMS derivatizations.
GC/MS analysisof ∆
9
-THC-11-oic acid in urine
188 Cannabinoids and their metabolites
GC analysisof cannabinoids...
... method
Qualitative analysis is made by the comparison of the retention time of a peak of a specimen
with that of the authentic standard and also by the con rmation of the absence of such a peak ... main tool for analysisof opiates
and their metabolites. However, at the present time, GC/MS is being widely used for opiate
analysis.
For HPLC analysisof the conjugated forms of opiates, the ... low levels of morphine starting from a large
amount of a specimen cannot be a proof of the intake of the drug. e level of morphine
in urine of healthy subjects determined by GC/MS was reported...
... action of methemo-
globin reductase (identical with cytochrome b
5
reductase requiring NADH as a cofactor) pres-
ent in mammalian red cells. e concentration of methemoglobin in blood of normal ...
nitromesitylene. The concentration of nitrite was 5 µg/mL for both chromatograms.
652 Nitrate and nitrite compounds
Except GC-NPD, GC-ECD can be used for analysisof nitrite and nitrate; but the ... appearance of many interfering peaks. By GC/MS in the EI mode, it
is di cult to detect the derivative, because of its lower sensitivity. Although there is a report [9]
dealing with sensitive GC/MS analysis...
... developed a modi cation of the methods, which enabled accurate determination
of blood Met-Hb even in the presence of high concentrations of CO-Hb by using about a
100-fold excess of potassium ferricynade ... Simultaneous determination of carboxyhemoglobin and methemoglo-
bin in victims of carbon monoxide poisoning. J Forensic Sci 25:546–549
6) Sato K, Katsumata Y, Aoki M et al. (1981) A practical method for ...
presence of a cryoprotectant for hemiglobin assay. Biochem Med Metab Biol 37:190–196
10) Sato K, Tamaki K, Tsutsumi H et al. (1990) Storage of blood for methemoglobin determination: comparison
of...
... aliquot of it is subjected to GC/MS analysis.
Cocaine and its metabolites
215
time of death nor those at the time of samplings. erefore, there are great variation in the fatal
levels of cocaine ... solvent mixture of chloroform
and isopropanol or ethanol should be used. e simultaneous analysis can be made using
chloroform/isopropanol (9:1) or (3:1), and using columns of Bond Elut Certify® ... rmation of a target compound is usually achieved by agreement of its mass spectrum with
that of the authentic standard. Since, with simultaneous use of a deuterated IS, a mass
spectrum of a target...
... 15 mg of free pentazocine. e solution is
transferred to a small glass centrifuge tube with a ground-in stopper, followed by addition of
several mg of solid K
2
CO
3
and 3 mL of chloroform. ... retention times of 3–7 min and 7–8 min, respectively. The amount of pentazocine
and IS spiked into 1 mL of blank whole blood or urine was equally 50 ng.
⊡ Figure 5.2
223
In two autopsy cases of pentazocine ... and GC/MS [8]. In this chapter, a simple method for GC/MS analysisof
pentazocine in human whole blood and urine is presented.
Structures of pentazocine and dextromethorphan (IS).
⊡ Figure 5.1
Reagents...
... one of the most powerful hallucinogenic
drugs of abuse. LSD was explosively abused in U.S.A. in the latter half of the 1960s. In Japan,
the amount of seizure of LSD is much smaller than that of ... hallucinogenic activity
of LSD was con rmed by Albert Hofmann who did synthesize the compound; the pharmaco-
logical activity can be obtained by oral administration of as small as 20–75 µg of LSD. e ab-
sorption ... solutions are combined. A er the pH of the solution is adjusted to 8.5,
the solution is extracted with an appropriate amount of chloroform four times. e combined
chloroform extract is evaporated...
... e
mass spectra of TFA derivatives of MDMA and its three metabolites obtained from the urine
specimen are shown in
> Fig. 7.5.
For the proof of the use of MDMA, detection of MDA along with ... stream of nitrogen and recon-
stituted in 0.1 mL of DPM (IS) solution. A 1-µL aliquot of it is injected into the GC/MS
system with a DB-17MS system
k
.
Assessment of the methods
EI mass spectra of ... with 2 mL of carbonate bu er solution (pH 10)
i
and extracted with 5 mL of chloroform/isopropanol (3:1, v/v).
234 3,4-Methylene dioxyamphetamines
Mass spectra of TFA derivatives of MDA, MDMA,...
... Modification of EMIT assay reagents for improved sensitivity and cost effective-
ness in the analysisof hemolyzed whole blood. J Anal Toxicol 16: 381–388
7) Sneath TC, Jain NC (1992) Evaluation of phencyclidine ... utilizing the ETS
®
analyzer and a 25-ng/
mL cutoff. J Anal Toxicol 16:107–108
8) Diosi DT, Harvey DC (1993) Analysisof whole blood for drugs of abuse using EMIT d.a.u. reagents and a Mon-
arch ... of a whole blood or urine specimen.
• 1 M NaHCO
3
solution: 8.4 g of NaHCO
3
is dissolved in distilled water to prepare 100 mL
solution.
• Chloroform/methanol (9:1, v/v): a 100-mL volume of...
... solution
b
. Many of the phenothiazine
drugs are in the forms of hydrochloride salt. For example, to prepare 1 mg/mL solution of the
free form of chlorpromazine, the amount of chlorpromazine ... various concentrations of
a target compound are prepared for a calibration curve.
Assessment of the method
All eleven kinds of phenothiazine drugs gave the base peaks of protonated molecular ... 10–100 fold.
k) As probable reasons of such a phenomenon, the slight thermal decomposition of the
authentic standard during the step of GC, and/or protection of the target phenothiazine
from...
... 2.2
HPLC and LC/MS analysis
269
Notes
a) When GC/MS, HPLC and LC/MS are compared for analysisof haloperidol and bromperi-
dol, the LC/MS seems of the best choice for their trace analysis. e HPLC ... excellent. e separation ability of GC or
GC/MS is much superior to that of HPLC or LC/MS.
HPLC and LC/MS analysis
Reagents and their preparation
e sources for acquisition of haloperidol, bromperidol ... volume of urine or blood, 0.05 mL IS and 0.5 mL of 1 M NaOH are placed in a 15-mL
volume glass centrifuge tube with a ground-in stopper and mixed well, followed by addi-
tion of 6 mL of the...
... control of her respiration and circulation, but she died in spite of the in-
tensive care on the second day. e analysisof blood sampled about 15 h a er ingestion showed
71.3 µg/mL of carbamazepine, ... tentative identi cation of drugs, a UV absorbance spectrum can
be measured together with the con rmation of coincidence of retention time of a test peak
with that of an authentic compound. ... Yashiki
Introduction
Many of antidepressants exert their e ects by inhibiting the reuptake of norepinephrine and
serotonin and by accerelating the release of them at synaptic terminals of neurons in the...
... application of a crude
specimen without any prior deproteinization process. “Internal surface reversed phase col-
umn” is one of the columns of this type. In this section, a method of LC/MS analysisof ... estazolam,
18: alprazolam, 19: tofisopam, 20: etizolam, 21: triazolam, 22: brotizolam.
⊡ Figure 4.1
GC/MS analysisof benzodiazepines in blood and urine
287
In the analysisof benzodiazepines by GC ... one of the serious social problems. In this chapter, a
GC/MS method for simultaneous analysisof 22 kinds of benzodiazepines listed in
> Table 4.1
is described. In addition, the LC/MS analysis...