Malaysian Journal of Analytical Sciences, Vol 26 No 5 (2022): 953 - 964

 

DISPERSIVE MICRO-SOLID-PHASE EXTRACTION (D-µ-SPE) WITH POLYPYRROLE-GRAPHENE OXIDE (PPY-GO) NANOCOMPOSITE SORBENT FOR THE DETERMINATION OF TETRACYCLINE ANTIBIOTICS IN WATER SAMPLES

 

(Pengekstrakan Fasa-Pepejal-Mikro Secara Serakan (D-µ-SPE) menggunakan Polipirol-Grafin Oksida (Ppy-GO) Penjerap Nanokomposit bagi Penentuan Antibiotik Tetrasiklin dalam Sampel Air)

 

Nurzaimah Zaini¹, Nor Suhaila Mohamad Hanapi¹*, Wan Nazihah Wan Ibrahim¹, Rozita Osman¹,

Sazlinda Kamaruzaman², Noorfatimah Yahaya³, Ahmad Lutfi Anis⁴

 

¹Faculty of Applied Sciences,

Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia

²Department of Chemistry,

Faculty of Science, Universiti Putra Malaysia, Serdang, Selangor, Malaysia

³Integrative Medicine Cluster, Advanced Medical and Dental Institute (AMDI),

Universiti Sains Malaysia, 13200 Bertam Kepala Batas, Penang, Malaysia

⁴Faculty of Applied Sciences,

Universiti Teknologi MARA, 94300 Kota Samarahan, Sarawak, Malaysia

 

^*Corresponding author: norsuhaila979@uitm.edu.my

 

 

Received: 18 May 2022; Accepted: 21 July 2022; Published:  30 October 2022

 

 

Abstract

Dispersive micro-solid-phase extraction (D-µ-SPE) method using polypyrrole-graphene oxide (PPy-GO) nanocomposite sorbent has been developed for the extraction and pre-concentration of tetracycline antibiotics (TCs) residues, namely oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC), demeclocycline (DMC) and doxycycline (DOC) in water samples prior to high-performance liquid chromatography-ultraviolet/diode array detector (HPLC-UV/DAD). The PPy-GO nanocomposite was prepared by in situ oxidative chemical polymerization. The effects of sample pH, a mass of sorbent, desorption solvent, extraction time and desorption time on the extraction of analytes were evaluated and optimized. Under the optimum conditions, the method demonstrated good linearity (R²=0.9989-0.9995) over a concentration range of 10-1000 µg L^-1. The limit of detection (LOD) was in the range of 4.9-8.7 µg L^-1 with satisfactory relative recoveries (80 – 105 %) and a good relative standard deviation (RSD) of ≤ 2.3 % (n = 3) was obtained. The method was successfully applied to river water and tap water samples. Results obtained using the developed method were compared with results previously reported using other SPE-based methods.

 

Keywords: tetracycline antibiotics, PPy-GO, dispersive micro-solid-phase extraction, liquid chromatography, water samples

 

Abstrak

Kaedah pengekstrakan fasa-pepejal-mikro secara serakan (D-µ-SPE) menggunakan penjerap nanokomposit polipirol- grafin oksida (PPy-GO) telah dibangunkan untuk pengekstrakan dan pra-pemekatan sisa antibiotik tetrasiklin (TCs), iaitu oksitetrasiklin (OTC), tetrasiklin (TC), klortetrasiklin (CTC), demeklosiklin (DMC) dan doksisiklin (DOC) di dalam sampel air sebelum kromatografi cecair berprestasi tinggi-pengesan tatasusunan ultraungu/diod (HPLC-UV/DAD). Nanokomposit PPy-GO telah disediakan melalui pempolimeran oksidatif kimia in situ. Kesan pH sampel, jisim penjerap, pelarut nyahjerapan, masa pengekstrakan dan masa nyahjerapan pada pengekstrakan analit telah dinilai dan dioptimumkan. Di bawah keadaan optimum, kaedah menunjukkan kelinearan yang baik (R²=0.9989-0.9995) dalam julat kepekatan 10-1000 µg L^-1. Had pengesanan (LOD) adalah dalam julat 4.9-8.7 µg L^-1 dengan pemulihan relatif yang memuaskan (80-105%) dan sisihan piawai relatif (RSD) yang baik sebanyak ≤ 2.3% (n = 3) telah diperoleh. Kaedah tersebut berjaya diaplikasikan pada sampel air sungai dan air paip. Keputusan yang diperoleh menggunakan kaedah yang dibangunkan dibandingkan dengan keputusan yang dilaporkan sebelum ini menggunakan kaedah berasaskan SPE yang lain.

 

Kata kunci: antibiotik tetrasiklin, Ppy-GO, pengekstrakan fasa-pepejal-mikro secara dispersif, kromatografi cecair, sampel air

 

 

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