Malaysian Journal of Analytical Sciences Vol 21 No 5 (2017): 1091 - 1100

DOI: https://doi.org/10.17576/mjas-2017-2105-11

 

 

 

A NEW AUTOMATED GAS CHROMATOGRAPHY/SOLID PHASE MICROEXTRACTION PROCEDURE FOR DETERMINING

α-FLUORO-β-ALANINE IN URINE

 

(Kaedah Baru Pengekstrakan Mikro Fasa Pepejal/Kromatografi Gas Berautomatik α-Fluoro-β-Alanina di dalam Urin)

 

Stefano Dugheri¹*, Alessandro Bonari², Ilenia Pompilio², Matteo Gentili³, Manfredi Montalti², Nicola Mucci², Giulio Arcangeli²

 

¹Laboratorio di Igiene e Tossicologia Industriale,

Azienda Ospedaliero-Universitaria Careggi, Firenze, Italy

²Dipartimento di Medicina Sperimentale e Clinica,

Università degli Studi di Firenze, Firenze, Italy

³Giotto Biotech Srl, Sesto Fiorentino, Italy

 

*Corresponding author:  stefano.dugheri@unifi.it

 

 

Received: 15 February 2017; Accepted: 16 June 2017

 

 

Abstract

In industrial hygiene, biomarkers maintain their promise to reveal the true extent of occupational exposure. The environmental limit values proposed by industrial hygienist associations are more than biological, health-based values indicating professional hazards to humans. High-throughput screening of samples is therefore the strategy of choice to detect occupational exposure biomarkers, yet it requires user-friendly apparatus that give relatively prompt results while ensuring high degrees of selectivity, precision, accuracy and automation, particularly in preparation processes. In light of the above, this contribution describes a novel gas chromatography/triple quadrupole mass  spectrometry/positive chemical ionisation approach for determining urinary α-fluoro-β-alanine, a metabolite of 5-fluorouracil, the most widely employed antineoplastic drug. In this new procedure chromatography’s sensitivity is combined with the user-friendliness of alkyl chloroformate/trialkyloxonium on-sample derivatizations followed by solid-phase microextraction sampling, to which is added the quantitative accuracy afforded using a specific isotope-labelled internal standard. The quantification limit for -fluoro--alanine was 25.4 µg/L. Intra- (3.8%) and inter-session (4.5%) repeatability was also evaluated. This method serves to identify suitable risk-control strategies for occupational hygiene conservation programs.

 

Keywords:  a-fluoro-b-alanine, solid phase microextraction, gas chromatography, occupational medicine

 

Abstrak

Dalam industri kesihatan, penanda biologi mengekalkan peranannya untuk mendedahkan sejauh mana keselamatan pekerjaan. Nilai had persekitaran yang dicadangkan oleh persatuan industri kesihatan melebihi daripada aspek biologi, iaitu tahap berasaskan kesihatan yang menunjukkan bahaya kepada manusia. Melalui saringan sampel, pemilihan strategi penting untuk mengesan pekerjaan yang terdedah kepada penanda biologi, maka alatan mesra pengguna yang memberikan keputusan segera disamping memastikan nilai kepilihan, kejituan, ketepatan dan bersifat automatik perlulah menjadi sebahagian proses tersebut. Sehubungan itu, sumbangan kajian ini adalah membincangkan kaedah novel kromatografi gas/spektrometri jisim caturkutub ganda tiga/pengionan kimia positif digunakan untuk penentuan α-fluoro-β-alanina di dalam urin, iaitu metabolit 5-fluorourasil yang digunakan secara meluas sebagai dadah antineoplastik. Melalui prosedur baru ini, sensitiviti kromatografi digabungkan bersama menggunakan kloroformat/trialkiloksonium di ikuti oleh pensampelan pengekstrakan mikro fasa pepejal, di mana ketepatan kuantitatif analisis didorong oleh penggunaan larutan piawai internal berlabel isotop. Had kuantifikasi a-fluoro-b-alanina ialah 25.4 µg/L. Kebolehulangan intra- (3.8%) dan inter- (4.5%) juga telah di uji. Kaedah ini menyediakan strategi kawalan penilaian risiko yang sesuai untuk program pemuliharaan kesihatan pekerjaan.      

 

Kata kunci:  a-fluoro-b-alanina, pengekstrakan mikro fasa pepejal, kromatografi gas, pekerjaan perubatan

 

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