scholarly journals Analytical confirmation of lethal heroin overdose by the use of liquid chromatography methods

2007 ◽  
Vol 64 (11) ◽  
pp. 739-743 ◽  
Author(s):  
Snezana Djordjevic ◽  
Vesna Kilibarda
Keyword(s):  
Liquid Chromatography ◽  
Ammonium Acetate ◽  
Physical Dependence ◽  
Post Mortem ◽  
Liquid Chromatography Mass Spectrometry ◽  
Mass Spectrometry Detection ◽  
Heroin Use ◽  
Liquid Liquid Extraction ◽  
The Brain

Background/Aim. Heroin is diacetylated morphine. Its ability to induce euphoria has led to its frequent abuse, giving rise to psychological and physical dependence. It has a short half-life, of approximately 2?6 min. In the brain, heroin undergoes deacetylation to 6-monoacetylmorphine (6?MAM) and morphine. Detection of 6-acetylmorphine in the urine is indicative of heroin use. The aim of this study was to compare sensitivity and reliability of two analytical methods, a multicolumn liquid chromatography system with UV scanning detector (HPLCUV) and liquid chromatography-mass spectrometry detection (LC-MS) in opiate determining in post mortem material. Methods. Post mortem samples (blood, urine and vitreous humor) were analyzed by liquid chromatography with UV and MS detection. The samples were prepared by liquid-liquid extraction with mixture chloroform-isopropanol (9:1). Separation was performed on C8 column with mobile phase composed of 55% acetonitrile-glacial acetic acid (99:1) and 45% 20 mM ammonium acetate. Results. The analysis of blood samples, urine, and eye liquid by the use of multicolumn HPLC-UV method confirmed the presence of morphine in the samples of blood and urine, codeine only in urine, and 6-MAM in the samples of urine and eye liquid. Using LC-MS method morphine was confirmed in all of the samples, while codeine was confirmed in urine and in the sample of eye liquid. In the samples of eye liquid and urine 6-MAM was confirmed. Conclusion. For determination of opiates in post mortem material LC-MS technique is more sensitive and reliable as compared to multicolumn liquid chromatography.

scholarly journals Liquid Chromatography with Mass Spectrometry—Detection of Lipophilic Shellfish Toxins

2005 ◽  
Vol 88 (5) ◽  
pp. 1371-1382 ◽  
Author(s):  
Lesley A Stobo ◽  
Jean-Pierre C L Lacaze ◽  
Alasdair C Scott ◽  
Susan Gallacher ◽  
Elizabeth A Smith ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Ammonium Acetate ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Quantitative Detection ◽  
Pecten Maximus ◽  
Mass Spectrometry Detection ◽  
Matrix Interferences

Abstract A rapid multiple toxin method based on liquid chromatography with mass spectrometry (LC/MS) was developed for the detection of okadaic acid (OA), dinophysistoxin-1 (DTX-1), DTX-2, yessotoxin (YTX), homoYTX, 45-hydroxy-YTX, 45-hydroxyhomo-YTX, pectenotoxin-1 (PTX-1), PTX-2, azaspiracid-1 (AZA-1), AZA-2, and AZA-3. Toxins were extracted from shellfish using methanol–water (80%, v/v) and were analyzed using a C8 reversed-phase column with a 5 mM ammonium acetate–acetonitrile mobile phase under gradient conditions. The method was validated for the quantitative detection of OA, YTX, PTX-2, and AZA-1 in 4 species (mussels, Mytilus edulis; cockles, Cerastoderma edule; oysters, Crassostrea gigas; king scallop, Pecten maximus) of shellfish obtained from United Kingdom (UK) waters. Matrix interferences in the determination of the toxins in these species were investigated. The validated linear range of the method was 13–250 μg/kg for OA, PTX-2, and AZA-1 and 100–400 μg/kg for YTX. Recovery and precision ranged between 72–120 and 1–22%, respectively, over a fortification range of 40–160 μg/kg for OA, PTX-2, and AZA-1 and 100–400 μg/kg for YTX. The limit of detection, reproducibility, and repeatability of analysis showed acceptable performance characteristics. A further LC/MS method using an alkaline hydrolysis step was assessed for the detection of OA, DTX-1, and DTX-2 on their esterified forms. In combination with the LC/MS multiple toxin method, this allows detection of all toxin groups described in Commission Decision 2002/225/EC.

Multiresidue analysis of pesticides in peanuts using modified QuEChERS sample preparation and liquid chromatography-mass spectrometry detection

2015 ◽  
Vol 7 (11) ◽  
pp. 4734-4739 ◽  
Author(s):  
Renata Pereira Lopes ◽  
Fabiano A. S. Oliveira ◽  
Fernando D. Madureira ◽  
Mauro Lúcio G. Oliveira ◽  
Gilsara Silva
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
Simultaneous Determination ◽  
Pesticide Residues ◽  
Liquid Chromatography Mass Spectrometry ◽  
Mass Spectrometry Detection ◽  
Multiresidue Analysis ◽  
Modified Quechers

A multiclass method has been optimized and validated for the simultaneous determination of 113 pesticide residues belonging to several classes in peanuts.

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