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Author:Rajamäki, Outi
Title:Huume- ja lääkeaineden GC-MS-analyysi StatSure Saliva SamplerTM -keräimellä kerätyistä sylkinäytteistä
The GC-MS analysis of drugs and pharmaceutical compounds in saliva collected by StatSure SalivaSamplerTM
Publication type:Master's thesis
Publication year:2012
Pages:viii + 84      Language:   fin
Department/School:Biotekniikan ja kemian tekniikan laitos
Main subject:Epäorgaaninen kemia   (Kem-35)
Supervisor:Kulmala, Sakari
Instructor:Langel, Kaarina ; Lillsunde, Pirjo
OEVS:
Electronic archive copy is available via Aalto Thesis Database.
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Location:P1 Ark Aalto  1918   | Archive
Keywords:quantification of drugs and medicines
validation
oral fluid
huumausaineet
lääkeainemääritys
GC-MS
validointi
sylkinäyte
Triton X-100
Abstract (eng): The purpose of the thesis was to develop and validate an analytical method for saliva samples collected with StatSureTM saliva samplers.
The thesis was a part of the DRUID project, within which the Alcohol and Drug Analytics Unit of the Finnish National Institute for Health took part.
The buffer solution of the saliva sampler contained high molecular detergents Triton X100 and IGPAL, which caused problems in gas chromatography analysis.
To eliminate this problem the aim was set to look for the optimal way to separate the buffer solution from the analytes.

The removal of the detergents was attempted by the use of Amberlite XAD resins or solid phase extraction.
The separation was studied with many different combinations of the washing and eluting solvents.
In addition, the impact of the derivatization agents on the detergents was studied.

For the method developed the gas chromatographic part of the analysis was divided into two parts: the benzodiazepines were analysed with GC-NICI-MS apparatus, and other drugs with GC-EI-MS.
For the latter purpose, analytes were derlvatized with MSTFA which also reacted with the detergents making them volatile.
MCX solid phase extraction columns were used for the pre-treatment in the determination of benzodiazepines.

The method was validated for 50 analytes.
The DRUID project requirements were not fulfilled as MDEA was not stable with this method and zopic1one and morphine didn't reach the determination limits.
The recovery was more than 75 % for the majority of the investigated drugs, but the recovery of the benzodiazepines was lower than that of the other drugs across the board.
In particular, the recovery of lorazepam and morphine were low, 35.36% and 44.74% respectively.
Abstract (fin): Diplomityön tarkoituksena oli kehittää ja validoida Terveyden ja hyvinvoinnin laitoksen päihdeanalytiikan yksikölle DRUID-projektia varten analyysimenetelmä StatSureTM -keräimillä kerätyille sylkinäytteille.
Keräimen puskuriliuoksen suurimolekyyliset detergentit Triton X-100 ja IGPAL aiheuttivat sellaisenaan ongelmia kaasukromatografianalyysissa, joten tutkimuksessa etsittiin optimaalisinta tapaa erottaa tutkittavat analyytit puskuriliuoksesta.

Detergenttien poistossa yritettiin hyödyntää Amberlite XAD-hartseja ja kiinteäfaasiuuttoa.
Molempien erotusmenetelmien yhteydessä tutkittiin erilaisia yhdistelmiä monista pesu- ja eluointiliuoksista.
Lisäksi tutkittiin analyyttien derivatisoinnissa käytettävien reagenssien vaikutusta detergentteihin.

Kehitetyn menetelmän kromatografinen analyysi jakautui kahteen osaan: bentsodiatsepiinit analysoitiin GC-NICI-MS -laitteistolla ja muut huumausaineet GC-EI-MS -laitteistolla.
Jälkimmäistä varten analyytit derivatisoitiin MSTFA:lla, jolloin myös detergenteistä muodostui haihtuvia johdannaisia.
Bentsodiatsepiinien määritystä varten esikäsittelyssä hyödynnettiin MCX-kiinteäfaasiuuttokolonneja.

Menetelmä validoitiin 50 analyytille.
DRUID-projektin edellyttämä MDEA ei ollut stabiili, eikä tsopiklonilla ja morfiinilla päästy projektin asettamiin määritysrajoihin.
Saanto oli valtaosalla tutkituista aineista yli 75 %, mutta bentsodiatsepiinien saanto jäi kauttaaltaan huonommaksi kuin muiden huumeiden.
Erityisesti loratsepaamin saanto jäi kovin pieneksi (35,36 %).
Muista huumeista morfiinin saanto jäi 44,74 %:iin.
ED:2012-09-17
INSSI record number: 45260
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