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Examination of Firearms Review: 2007 to 2010 - Interpol

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used most frequently [375].<br />

A comparative study was made between LLE and direct injection for the<br />

LC-MS/MS detection <strong>of</strong> 34 diuretics and 9 other doping agents in urine [376].<br />

With a 25-fold dilution <strong>of</strong> the urine samples, the problems <strong>of</strong> retention time<br />

shifting and ion-suppression in direct injection were improved compared with<br />

the undiluted samples, with results comparable <strong>to</strong> those obtained from LLE. A<br />

fully au<strong>to</strong>mated method based on UPLC-MS/MS for the analysis <strong>of</strong> 130<br />

substances by direct injections <strong>of</strong> urine samples has been developed for three<br />

different classes <strong>of</strong> doping agents: diuretics, central nervous system stimulants<br />

(CNS stimulants), and opiates [377].<br />

Direct analysis <strong>of</strong> urine samples by UPLC-MS/MS has been developed for<br />

quantitation <strong>of</strong> salbutamol [378]. With salbutamol-d6 as internal standard<br />

followed by dilution with ultrapure water (1:1), the LOQ was 200 ng/mL. A<br />

quantitative LC-MS/MS method <strong>to</strong> detect altizide, hydrochlorothiazide and their<br />

common metabolites (chlorothiazide and<br />

4-amino-6-chloro-1,3-benzenedisulphonamide) was developed, and the<br />

concentrations ranges were found <strong>to</strong> be between 41-239 and 60-287 ng/mL<br />

after altizide and hydrochlorothiazide administration, respectively [379]. The<br />

study also showed that 4-amino-6-chloro-1,3-benzenedisulphonamide is an<br />

important target compound <strong>to</strong> detect usage <strong>of</strong> thiazide diuretics. CE coupled<br />

with field-amplified sample stacking (FASS) has been reported for the<br />

simultaneous determination <strong>of</strong> strychnine and brucine residues in human urine,<br />

with detection limits <strong>of</strong> 2 and 2.5 ng/mL, respectively [380].<br />

The administration <strong>of</strong> glycerol <strong>to</strong> endurance athletes results in an increased<br />

fluid retention and improved performance, particularly under hot and humid<br />

conditions. A quantitative method was established using a GC/iso<strong>to</strong>pe-dilution<br />

MS-based approach, with an LOD <strong>of</strong> 0.3 µg/mL [381]. A 200 µg/mL threshold<br />

for glycerol levels in urine is suggested based on the analysis <strong>of</strong> 1039 doping<br />

control samples. An important aspect <strong>of</strong> doping research is the rapid<br />

implementation <strong>of</strong> tests for emerging drugs with potential for misuse in<strong>to</strong><br />

routine doping control assays. The mass spectrometric fragmentation <strong>of</strong> four<br />

new emerging drug candidates: GW501516 (PPAR-delta-agonists), S-107 and<br />

JTV-519 (ryanodine-calstabin-complex stabilizers), and S-40503 (selective<br />

androgen recep<strong>to</strong>r modula<strong>to</strong>rs) were studied, and a screening and<br />

confirmation procedure was established for the analysis <strong>of</strong> these drugs in<br />

659

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