... 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 ... 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 ... 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...
... to dryness.
ii. Solid-phase extraction [10]
i. A 2-mL volume of the hydrolyzed urine obtained a er step i) of the above procedure is
mixed with a xed amount of IS
h
, and poured into a Bond ... cannabinoids exist in the carboxylated form. ey are easily de-
carboxylated at 250 °C.
d) ere are reviews dealing with GC/MS analysisof ∆
9
-THC-11-oic acid in human urine
[15, 16].
e) A method of ... 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 ... the oxidoreductive potential of the hydroxyl group of the
phenol moiety, it is not suitable for analysis codeine or M-3-G. For cautions and cuto values
upon detection of trace levels of morphine, ... 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...
... vortex mixed for 1 min.
vi. A er centrifugation at 3,000 rpm for 2 min, 1- or 4-µL of the supernatant solution is in-
jected into GC.
vii. e above procedure consists of the oxidation of nitrite ... should be worn, considering
the rare accident of leakage of the mixture due to the exothermic phenomenon. However
the author et al. have no experience of such accidents.
References
1) Haddad LM, ... the mixture, appreciable heat is produced. e addition
of the acid should be as slow as possible, followed by airtight capping of the polypropylene
tube. Upon nitri cation with vortex-mixing,...
... and
Extrelut®.
b) e Bond Elut Certify®
column is composed of a mixture of non-polar phase and a cation
exchanger phase; the mechanisms are reversed-phase extraction plus cation-exchanging ... polar 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 ... conversion of amounts of EME and BE into those of
cocaine
Poisoning case
209
a) Procedure I (Bond Elut Certify
®
) [6–8]
i. Extraction from urine and derivatization
i. A 5-mL volume of urine is mixed...
... 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. ... Toxicology for Clinical,
Forensic and Pharmaceutical Chemists. Walter de Gruyter, Berlin, pp 707–718
10) Association of Medical Examiners, NAME, Pediatric Toxicology Registry, USA (1994) Dextromethorphan ... [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 and...
... 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 ... tartarate extract 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 ... manufacturers).
Developing solvents: (A) acetone/chloroform (4:1, v/v); (B) chloroform/methanol/n-hex-
ane (4:2:1, v/v).
Assessment of the method
e R
f
values of LSD were 0.29 with the (A) solvent system...
... metabolite of MDMA [6–9]. For more reliable and
e ective proof of the use of MDAs, their metabolites with the cleavage of methylenedioxy
rings, such as HMMA, HMA and 4-hydroxy-3-methoxyethylamphetamine, ... procedure.
ii. Extraction
Liquid-liquid extraction:
i. e above hydrolyzed solution is mixed with 2 mL of carbonate bu er solution (pH 10)
i
and extracted with 5 mL of chloroform/isopropanol ... analyses of MDAs in the forms of
tablets and those for GC/MS analysisof MDAs and their main metabolites 4-hydroxy-3-me-
thoxymethamphetamine ( HMMA) and 4-hydroxy-3-methoxyamphetamine ( HMA) in urine...
... 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 1000 chemistry analyzer. J Anal Toxicol ... gentle streams of nitrogen at
room temperature.
ii. A 1-mL volume of blank blood or distilled water is added to each test tube and mixed on
the vortex mixer
h
.
iii. Each mixture is then processed ... Phencyclidine-related deaths: a report of nine fatal cases. J Anal Toxicol
3:199–201
253
10) ElSohly MA, Lee LF, Halzhauer LB et al. (2001) Analysisof urine samples in cases of alleged sexual assault: case
history....
... 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 ... concentrations of the com-
pound are prepared to construct a calibration curve, consisting of drug concentration on
the horizontal axis and of peak area ratio of a drug to IS on the vertical axis. ... appropriate amount of IS, 3 mL distilled water and
0.5 mL of 1 M sodium bicarbonate solution. A er well mixing, the mixture is centrifuged
at 3,000 rpm for 10 min. For IS, one of other phenothiazine...
... 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 mixture ... aqueous phase
is again washed with 1 mL of the mixture of n-hexane/isopropanol by shaking it for 30 s.
iv. A er centrifugation at 600 g for 5 min, 1.2 mL of the lower aqueous phase is transferred ... glass centrifuge tube with a ground-in stopper, followed by addition of 0.2 mL
of 1 M NaOH and 1 mL of the n-hexane/isopropanol mixture, and vigorous shaking for 30 s.
v.
A er centrifugation at...
... mobile phase (B). With the use of the Eclipse XDB-C
8
column, the peak top of nortriptyline (D) could be separated from that of amoxapine (E), but
major parts of their peaks could not be separated. ... higher to
enable detection of the peak of lofepramine.
Poisoning cases, and toxic and fatal concentrations
In > Table 3.1, the therapeutic and toxic blood concentrations of each compound are shown ... 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,...
... spectra of triazolam, 4-hydroxytriazolam and α-hydroxytriazolam.
⊡ Figure 4.2
Toxic and fatal concentrations
290 Benzodiazepines
Mass chromatograms of triazolam, 4-hydroxytriazolam, α-hydroxytriazolam ... the decomposition of drugs due to
heat frequently takes place. e decomposition is marked especially for oxazolam, cloxazolam,
mexazolam, utazolam and haloxazolam having oxazolo rings in their ... 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 analysis of...