Human serum analysis

Sjodin A, Thuresson K, Hagmar L, et al. 1999b. Occupational exposure to polybrominated diphenyl ethers at dismantling of electrons. Ambient air and human serum analysis. Organohalogen Compounds 43 447-451. 

Human serum analysis Eluent A (0.05 M perchloric acid ACN = 60 40)/eluent B (0.05 M perchloric acid ... 

Quero C, Colome N, Prieto MR, Carrascal M, Posada de la Paz M, Gelpi E, Abian J (2004) Determination of protein markers in human serum analysis of protein expression in toxic oil syndrome studies. Proteomics, 4 303-315. 

T. Hyotylainen, T. Andersson and M. E. Riekkola, Eiquid cliromatographic sample cleanup coupled on-line with gas chromatography in the analysis of beta-blockers in human serum and urine , 7. Chromatogr. Sci. 35 280-286 (1997). 

Comprehensive two-dimensional GC has also been employed for the analysis of pesticides from serum, which, although not strictly a forensic analytical problem , provides an example of the promise of this technique to forensic applications, such as the analysis of drugs of abuse (40). Two-dimensional gas chromatograms of a 17-pesticide standard and an extract from human serum are shown in Figure 15.13. The total analysis time of about 5 min, high peak capacity and the separation of all... 

Methyl parathion was determined in dog and human serum using a benzene extraction procedure followed by GC/FID detection (Braeckman et al. 1980, 1983 DePotter et al. 1978). An alkali flame FID (nitrogen-phosphorus) detector increased the specificity of FID for the organophosphorus pesticides. The detection limit was in the low ppb (pg/L). In a comparison of rat blood and brain tissue samples analyzed by both GC/FPD and GC/FID, Gabica et al. (1971) found that GC/FPD provided better specificity. The minimum detectable level for both techniques was 3.0 ppb, but GC/FPD was more selective. The EPA-recommended method for analysis of low levels (<0.1 ppm) of methyl parathion in tissue, blood, and urine is GC/FPD for phosphorus (EPA 1980d). Methyl parathion is not thermally stable above 120 °C (Keith and Walters 1985). 

GC/MS has been employed by Demeter et al. (1978) to quantitatively detect low-ppb levels of a- and P-endosulfan in human serum, urine, and liver. This technique could not separate a- and P-isomers, and limited sensitivity confined its use to toxicological analysis following exposures to high levels of endosulfan. More recently, Le Bel and Williams (1986) and Williams et al. (1988) employed GC/MS to confirm qualitatively the presence of a-endosulfan in adipose tissue previously analyzed quantitatively by GC/ECD. These studies indicate that GC/MS is not as sensitive as GC/ECD. Mariani et al. (1995) have used GC in conjunction with negative ion chemical ionization mass spectrometry to determine alpha- and beta-endosulfan in plasma and brain samples with limits of detection reported to be 5 ppb in each matrix. Details of commonly used analytical methods for several types of biological media are presented in Table 6-1. 

Murkovic, M., Adam, U., and Pfannhauser, W., Analysis of anthocyane glycosides in human serum, Fresenius J. Anal. Chem., 366, 379, 2000. 

Hanai, T., Miyazaki, R., and Kinoshita, T., Quantitative analysis of human serum albumin-drug interactions using reversed phase and ion-exchange liquid chromatography, Anal. Chim. Acta, 378, 77, 1999. 

Kilar, E and Hjerten,S., Fast and high resolution analysis of human serum transferrin by high performance isoelectric focusing in capillaries, Electrophoresis, 10, 23, 1989. 

Thormartn, W., Meier, R, Marcolli, C., and Binder, F., Analysis of barbiturates in human serum and urine by high-performance capillary electrophoresis-micellar electrokinetic capillary chromatography with on-column multiwavelength detection, /. Chromatogr., 545, 445, 1991. 

Urdea, M. S., et al. (1987). A novel method for the rapid detection of specific nucleotide sequences in crude biological samples without blotting or radioactivity application to the analysis of hepatitis B virus in human serum. Gene 61, 253-264. 

Figure 12.5 illustrates the problem of using human serum digest analysis. The digest was fractionated using a 2.1 x 150 mm C18 column at pH 10 (50 J,L serum... 

FIGURE 12.5 Human serum tryptic digest analysis. Fractionation in the first LC dimension was performed using a C18 column at pH 10. Fractions were analyzed using NanoEase 0.3 x 150 mm Atlantis d18 column. Approximately 66 lg (400 pmole of semm albumin peptides) was injected on column. Arrow points to a selected albumin peptide illustrating a local column mass overloading. Ten-5mm wide fractions were collected in 1st LC dimension. 

Bjorhall, K., Miliotis, T., Davidsson, P. (2005). Comparison of different depletion strategies for improved resolution in proteomic analysis of human serum samples. Proteomics 5, 307-317. 

Mass spectrometry (MS) is also being used to add another dimension of analysis to achiral-chiral analysis. Recently, an achiral-chiral column-switching LC/LC-MS/MS method was reported for the pindolol enantiomers in human serum (Motoyama et al., 2002) and phenprocoumon metabolites (Kammerer et al., 1998). For analytes that have very poor chromophores or cannot naturally fluoresce, MS detection can be more sensitive for the underivatized form of the analyte. Also, MS detection can be particularly useful when very similar analytes that differ in mass (such as some amino acids and metabolites) cannot be satisfactorily separated chromatographically,... 

Recently, sulfur mustard has been shown to alkylate a cysteine residue in human serum albumin (10). The site of alkylation was identified in a tryptic digest of albumin from blood exposed to [14C]sulfur mustard. A sensitive method for its analysis was developed based on Pronase digestion of alkylated albumin to the tripeptide S-[2-[(hydroxyethyl)thio]ethyl-Cys-Pro-Phe, and detection using micro-LC-MS-MS. In vitro exposure of human blood to > 10 nM sulfur mustard could be detected employing this method. The analytical procedure was successfully applied to albumin samples from Iranian casualties of the Iraq-Iran war. 

Mason, A.B., Halbrooks, P.J., James, N.G., Connolly, S.A., Larouche, J.R., Smith, V.C., MacGillivray, R.T.A. and Chasteen, N.D. (2005) Mutational analysis of C-lobe ligands of human serum Transferrin insights into the mechanism of iron release, Biochemistry, 44, 8013-8021. 

A. A. Bhattacharya, T. Grime, S. Curry, Crystallographic Analysis Reveals Common Modes of Binding of Medium and Long-Chain Fatty Acids to Human Serum Albumin , J. Mol. Biol. 2000, 303,121-132. 

Waschgler R, Hubmann MR, Conca A, MoU W, Konig P. 2002. Simultaneous quantification of citalopram, clozapine, fluoxetine, norfluoxetine, maprotiline, desmethylmaprotiline and trazodone in human serum by HPLC analysis. Int J Clin Pharmacol Ther 40(12) 554-559. 

Hansen G, Christensen P, Tuchsen E, Lund T. 2004. Sensitive and selective analysis of coenzyme QlO in human serum by negative APCI LC-MS. Analyst 129 45. 

Spell JC, Srinivasan K, Stewart JT, Bartlett MG. 1998. Supercritical fluid extraction and negative ion electrospray liquid chromatography tandem mass spectrometry analysis of phenobarbital, butalbital, pentobarbatal and thiopentoal in human serum. Rapid Commun Mass Spectrom 12 890. 

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