Malaysian Journal of Analytical Sciences Vol 19 No 4 (2015): 715 - 721

 

 

 

ANALYTICAL METHOD DEVELOPMENT FOR IMAZAPIC HERBICIDE USING HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

 

(Pembangunan Kaedah Analitikal Bagi Racun Rumpai Imazapic Menggunakan Kromatografi Cecair Prestasi Tinggi)

 

Anis Zakiah Mazlan^1*, Hazilia Hussain¹, Mohamed Azwan Mohamed Zawawi², Mehdi Sameni¹

 

¹Faculty of Health Sciences,

Universiti Teknologi MARA, Kampus Puncak Alam,

42300 Bandar Puncak Alam, Selangor Darul Ehsan, Malaysia

²Faculty of Engineering,

Universiti Putra Malaysia, 43400, Serdang, Selangor Darul Ehsan, Malaysia

 

*Corresponding author: aniszakiah89@yahoo.com

 

 

Received: 23 November 2014; Accepted: 27 June 2015

 

 

Abstract

A reliable method using High Performance Liquid Chromatography (HPLC) was developed for the optimization of imazapic herbicide extraction and clean-up method from water.  For this purpose, an Agilent HPLC 1200 Series fitted with a UV detector was used. The column used was a Zorbax StableBond C₁₈ (4.6mm x 250mm I.D., 5µm particle size). For the extraction and clean-up procedure, a solid-phase extraction (SPE) method was applied. Two types of cartridges were chosen namely styrene-divinylbenzene polymer bond elut PPL (PPL) and octadecyl/ silica bond elut C₁₈ (C₁₈), for comparison of the recovery performance. Good resolution of imazapic was optimum at l=252nm wavelength. The mobile phase was acetonitril: ultra-pure water (pH 3.0), in the ratio of 45:55. The flow rate of the mobile phase and injection volume were 1.2 mL/min and 20 µL, respectively.  Efficacy of extraction method used was determined through recovery test conducted using water samples spiked with imazapic standard. The recovery was 112% and 73% for C₁₈ cartridge and 10.35% and 10.14% for PPL at concentration of 2 and 10 mg L^-1, respectively. In conclusion, C₁₈ cartridge was chosen as the best cartridge for the extraction, clean-up method and determination of imazapic in water.

 

Keywords: bond elut C₁₈ (C₁₈), bond elut PPL (PPL), High Performance Liquid Chromatography (HPLC), imazapic, solid -phase extraction (SPE)

 

Abstrak

Satu kaedah boleh dipercayai menggunakan Kromatografi Cecair Prestasi Tinggi (KCPT) telah dibangunkan untuk mengoptimumkan pengekstrakan dan prosedur pembersihan racun rumpai imazapic dari sampel air. Untuk tujuan ini, sebuah Agilent KCPT 1200 Siri dilengkapi dengan pengesan UV telah digunakan. Turus yang digunakan adalah Zorbax StableBond C18 (4.6mm x 250mm ID, saiz zarah 5μm). Untuk pengekstrakan dan prosedur pembersihan, kaedah pengekstrakan fasa pepejal (SPE) telah digunakan. Dua jenis kartrij telah dipilih iaitu stirena-divinylbenzene bond elut polimer PPL (PPL) dan oktadesil / silika bond elut C₁₈ (C₁₈) bagi membandingkan prestasi pemulihan mereka. Resolusi imazapic yang baik adalah optimum pada ketika panjang gelombang l=252nm. Fasa bergerak adalah acetonitril: air ultra-tulen (pH 3.0), dalam nisbah 45:55. Kadar aliran dan jumlah suntikan ialah 1.2 mL/min dan 20 μL, masing-masing. Keberkesanan kaedah pengekstrakan yang digunakan ditentukan melalui ujian pemulihan yang dijalankan menggunakan sampel air yang dicampurkan dengan standard imazapic. Keputusan bagi kadar pemulihan adalah 112% dan 73% untuk kartrij C₁₈ dan 10.35% dan 10.14% untuk PPL pada kepekatan 2 dan 10 mg L^-1, masing-masing. Kesimpulannya, kartrij C₁₈ dipilih sebagai kartrij yang terbaik untuk pengekstrakan, kaedah pembersihan dan penentuan imazapic dalam air.

 

Kata kunci:  Bond elut C₁₈ (C₁₈), Bond elut PPL (PPL), Imazapic, Kromatografi Cecair prestasi Tinggi (KCPT), Pengekstrakan fasa pepejal (SPE).

 

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