Abstract & References Vol 24 No 6 (2020)

Malaysian Journal of Analytical Sciences Vol 24 No 6 (2020): 927 - 939

OPTIMISATION AND VALIDATION OF ULTRAHIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR QUANTIFICATION OF 25-HYDROXYVITAMIN D IN MATERNAL PLASMA

(Pengoptimuman dan Pengesahan Kaedah Kromatografi Cecair Berprestasi Ultra Tinggi untuk Kuantifikasi 25-hidroksivitamin D dalam Plasma Ibu Mengandung)

Siew Siew Lee and Su Peng Loh*

Department of Nutrition,

Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia

*Corresponding author: sploh@upm.edu.my

Received: 19 August 2020; Accepted: 25 October 2020; Published: 10 December 2020

Abstract

This study aimed to optimise and validate a simple and efficient sample preparation and extraction method for the quantification of 25-hydroxyvitamin D (25OHD) in the maternal plasma sample. Different sample preparation methods and precipitation reagent-to sample ratio used by previous studies were compared. An ultrahigh performance liquid chromatography method was developed and validated for simultaneous quantification of 25OHD₂ and 25OHD₃. The chromatographic separation was achieved using the COSMOCORE 2.6Cholester Column and methanol and 0.1% formic acid (79:21, %v/v) as mobile phase at a flow rate of 0.3 mL/min and diode array detection at 264 nm. The results demonstrated that a recovery of approximately 100% could be achieved by extracting samples using 1 mL of hexane, vortex for 10s and a total number of three extraction steps. The precipitation reagent-to-sample ratio of 2.8 was optimum for the quantification of 25OHD₂ and 25OHD₃ in a pooled maternal sample. The value obtained for validation parameters meets the criteria of the Recommendations and Acceptance Criteria for Bioanalytical Method Validation by the Food and Drug Administration. The results showed that this method could be applied for routine quantification of 25OHD, particularly in the maternal plasma sample.

Keywords: 25-hydroxyvitamin D, maternal, ultrahigh performance liquid chromatography, extraction

Abstrak

Kajian ini bertujuan mengoptimumkan dan mengesahkan kaedah penyediaan dan pengekstrakan yang mudah dan cekap untuk pengkuantitian 25-hidroksivitamin D (25OHD) di dalam sampel plasma ibu mengandung. Kaedah kromatografi cecair berprestasi ultra tinggi telah dibangunkan dan disahkan untuk pengkuantitian 25OHD₂ and 25OHD₃ secara serentak. Pemisahan kromatografi telah dicapai melalui turus COSMOCORE 2.6Cholester dan metanol: 0.1% asid formik (79:21, %v/v) sebagai fasa bergerak pada kadar aliran 0.3 mL/min dan pengesahan susunan diod pada 264 nm. Keputusan kajian menunjukkan bahawa kaedah pengekstrakan terbaik yang memberi kadar pemulihan yang hampir dengan 100% adalah mengekstrak sampel dengan menggunakan 1mL heksana, vorteks selama 10 s dan sejumlah 3 kali bagi langkah pengekstrakan. Kadar reagen pemendakan kepada sampel sebanyak 2.8 adalah optimum bagi pengekstrakan 25OHD₂ dan 25OHD₃ dalam sampel plasma ibu mengandung. Nilai yang diperolehi untuk parameter validasi adalah memenuhi kriteria cadangan dan kriteria penerimaan untuk pengesahan kaedah bioanalitikal oleh pentadbiran makanan dan ubat-ubatan (FDA). Hasil kajian menunjukkan bahawa kaedah yang diperolehi boleh diguna untuk rutin pengkuantitian 25OHD dalam sampel plasma, terutamanya sampel plasma dari ibu mengandung.

Kata kunci: 25-hidroksivitamin D, ibu mengandung, kromatografi cecair berprestasi ultra tinggi, pengekstrakan

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