handbook of practical analysis

... 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 of analysis of alkyl ... eld of forensic toxicology. In this chapter, the methods for analysis of the compounds by headspace (HS)-gas chromatography (GC) and liquid-liquid extraction-GC are presented. Determination of...

Ngày tải lên: 18/10/2013, 00:15

... Paasivirta J et al. (1981) Trace Analysis of 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...

Ngày tải lên: 18/10/2013, 00:15

... GC/MS analysis of ∆ 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 analysis of 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 analysis of ∆ 9 -THC-11-oic acid in urine 188 Cannabinoids and their metabolites GC analysis of cannabinoids...

Ngày tải lên: 24/10/2013, 19:15

... 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 analysis of opiates and their metabolites. However, at the present time, GC/MS is being widely used for opiate analysis. For HPLC analysis of 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...

Ngày tải lên: 24/10/2013, 19:15

... 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 analysis of 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...

Ngày tải lên: 24/10/2013, 19:15

... 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...

Ngày tải lên: 24/10/2013, 19:15

... 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...

Ngày tải lên: 29/10/2013, 01:15

... 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 analysis of pentazocine in human whole blood and urine is presented. Structures of pentazocine and dextromethorphan (IS). ⊡ Figure 5.1 Reagents...

Ngày tải lên: 29/10/2013, 02:15

... 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...

Ngày tải lên: 08/11/2013, 01:15

... 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,...

Ngày tải lên: 08/11/2013, 01:15

... Modification of EMIT assay reagents for improved sensitivity and cost effective- ness in the analysis of 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) Analysis of 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...

Ngày tải lên: 08/11/2013, 01:15

... 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...

Ngày tải lên: 15/12/2013, 12:15

... 2.2 HPLC and LC/MS analysis 269 Notes a) When GC/MS, HPLC and LC/MS are compared for analysis of 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...

Ngày tải lên: 15/12/2013, 12:15

... control of her respiration and circulation, but she died in spite of the in- tensive care on the second day.  e analysis of 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...

Ngày tải lên: 15/12/2013, 12:15

... 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 ... estazolam, 18: alprazolam, 19: tofisopam, 20: etizolam, 21: triazolam, 22: brotizolam. ⊡ Figure 4.1 GC/MS analysis of benzodiazepines in blood and urine 287 In the analysis of benzodiazepines by GC ... one of the serious social problems. In this chapter, a GC/MS method for simultaneous analysis of 22 kinds of benzodiazepines listed in > Table 4.1 is described. In addition, the LC/MS analysis...

Ngày tải lên: 15/12/2013, 12:15

Ngày tải lên: 15/12/2013, 12:15

Ngày tải lên: 15/12/2013, 12:15

Ngày tải lên: 15/12/2013, 12:15

Ngày tải lên: 15/12/2013, 12:15

Ngày tải lên: 15/12/2013, 12:15