VALIDASI METODE ANALISIS RESIDU ANTIBIOTIK ENROFLOKSASIN DALAM SUSU MENGGUNAKAN KROMATOGRAFI CAIR KINERJA TINGGI (KCKT)

Prima Mei Widiyanti, Raphaella Widiastuti, Mirnawati B Sudarwanto, Etih Sudarnika

Abstract

Enrofloksasin merupakan satu dari jenis antibiotik golongan fluorokuinolon yang digunakan untuk terapi pada hewan. Enrofloksasin memiliki spektrum luas, sehingga efektif untuk pengobatan penyakit infeksi bakteri Gram positif dan Gram negatif. Residu antibiotik enrofloksasin dalam susu dapat mempengaruhi kualitas produk dan kesehatan manusia. Penelitian ini bertujuan untuk validasi metode deteksi residu antibiotik enrofloksasin dalam susu menggunakan metode kromatografi cair kinerja tinggi (KCKT). Tahapan validasi metode deteksi residu antibiotik enrofloksasin dalam susu menggunakan HPLC meliputi spesifisitas, akurasi, presisi, linieritas, limit of detection (LOD), dan limit of quantitation (LOQ). Hasil validasi metode menunjukkan spesifisitas yang baik. Hasil akurasi yang diperoleh menunjukkan persentase rataan 98.86% dan presisi dengan nilai relative standard deviation (RSD) adalah 3.75% serta linieritas dengan nilai koefisien determinasi (R2)=0.999. Hasil LOD adalah 11.44 ppb dan LOQ adalah 15.28 ppb. Validasi metode analisis antibiotik enrofloksasin menggunakan HPLC pada semua parameter validasi menunjukkan hasil yang baik sesuai persyaratan regulasi. Berdasarkan hasil tersebut, maka metode dapat digunakan untuk menganalisis residu antibiotik enrofloksasin dalam sampel susu secara kuantitatif untuk menjamin keamanan pangan asal hewan demi peningkatan kesehatan masyarakat.

Keywords

antibiotik, enrofloksasin , KCKT, validasi, susu.

Full Text:

PDF

References

Ambarwati, Ariyani N, Palupi MF. 2013. Validasi metode spektrofotometri pada uji kadar sediaan injeksi obat hewan enrofloksasin. JSV. 31(2):266-273.

[APVMA] Australian Pesticides and Veterinary Medicines Authority. 2014. Validation of analytical methods for active constituents and agricultural products. [diunduh 2020 Jan 9]. Tersedia pada: https://apvma.gov.au/node/1048.

Ardianingsih R. 2009. Penggunaan high performance liquid chromatography (HPLC) dalam proses analisa deteksi ion. Berita Dirg. 10(4):101-104.

As ZA, Hardiono, Syarifudin A. 2014. Percobaan produksi biogas dari kotoran sapi dan kotoran ayam dengan penambahan enzim papain. J Kes Ling. 11(1):177-183.

Asredie T, Engdaw TA. 2015. Antimicrobial residues in cow milk and its public health significance. J Dairy Food Sci. 10(2):147-153.

Aulia SS, Sopyan I, Muchtaridi. 2017. Penetapan kadar simvastatin menggunakan kromatografi cair kinerja tinggi (KCKT):review. Farmaka. 14(4):70-78.

Babaahmady E, Khosravi A. 2011. Toxicology of baytril (enrofloxacin). Afr J Pharm Pharmacol. 5(18):2042-2045.

Bacanli M, Basaran N. 2019. Importance of antibiotic residues in animal food. J Food Chem Tox. 125:462-466.

[BSN] Badan Standardisasi Nasional. 2011. SNI 3141.1-2011 tentang Susu Segar bagian 1: Sapi. Jakarta: BSN.

Bilandzic N, Kolanovic BS, Varenina I, Jurković Z. 2011. Concentrations of veterinary drug residues in milk from individual farms in Croatia. Mljekarstvo. 61(3):260-267.

Cinquina, AL, Roberti P, Giannetti L, Longo F, Draisci R, Fagiolo A, Brizioli NR. 2003. Determination of enrofloxacin and its metabolite ciprofloxacin in goat milk by high-performance liquid chromatography with diode-array detection. J Chrom. 987:221-226.

Dianawati M, Mulijanti SL. 2015. Peluang pengembangan biogas di sentra sapi perah. J Lit Pertanian. 34(3):125-134.

[EC] The European Commission. 2010. Commission regulation (EU) No 37/2010 on pharmacologycally active substances and their classification regarding maximum residue limits in foodstuffs of animal origin [Internet]. [diunduh 2019 Mei 20]. Tersedia pada: https://ec.europa.eu/health/sites/health/files/files/eudralex/vol-5/reg_2010_ 37/ reg_2010_37_en.pdf.

[FDA] Food and Drug Administration. 2019. Guidelines for the validation of chemical methods in food, feed, cosmetics, and veterinary products [Internet]. [diunduh 2020 Feb 10]. Tersedia pada: https://www.fda.gov/media/81810/download.

Hruba H, Abdelsalam EEE, Anisimov N, Bandouchova H, Havelkova B, Heger T, Kanova M, Kovacova V, Nemcova M, Piacek V, et al. 2019. Reproductive toxicity of fluorokuinolones in birds. BMC Vet Res. 15(209):1-8.

Jayalakshmi K, Paramasivam M, Sasikala M, Tamilam TV, Sumithra A. 2017. Review on antibiotic residues in animal products and its impact on environments and human health, J Entomol Zool Std. 5(3):1446-1451.

Jevinova P, Dudrikova E, Sokol J, Nagy J, Mate D, Pipova M, Cabadaj R. 2003. Determination of oxytetracycline in milk with the use of HPLC method and two microbial inhibition assays. Bull Vet Inst Pulaway. 47:211-216.

Lestari F. 2007. Bahaya Kimia: Sampling dan Pengukuran Kontaminan Kimia di Udara. Jakarta (ID): EGC.

Mahmood T, Abbas M, Ilyas S, Fzal N, Nawaz R. 2016. Quantification of fluoroquinolon (enrofloxacin, norfloxacin and ciprofloxacin) residues in cow milk. IJCBS. 10:10-15.

Mellado M, Garcia JE, Deras FGV, Santiago MA, Mellado J, Gaytan LR, Garcia OA. 2018. The effect of periparturient events, mastitis, lameness and ketosis, on reproductive performance of Holstein cows in a hot environment. Austral J Vet Sci. 50:1-8.

Moghadam MM, Amiri M, Riabi HR, Riabi HR. 2016. Evaluation of antibiotic residues in pasteurized and raw milk distributed in the south of Khorasan-e Razavi province, Iran. J Clin Diagn Res. 10(12):31-35.

Mohammed HA, Abdou AM, Eid AM, Zakaria AM. 2016. Rapid test for detection of enrofloxacin residues in liquid milk. BVMJ. 30(1):97-103.

Moharana B, Venkatesh PK, Preetha SP, Selvasubramanian S. 2015. Quantitation of enrofloxacin residues in milk sample using RP-HPLC. World J Pharm Sci. 4(10):1443-1450.

Mourad G, Bettache G, Medjekal S. 2014. Composition and nutritional value of raw milk. Issues Biol Sci Pharm Res. 2(10):115-122.

Navratilova P, Borkovcova I, Vyhnalkova J, Vorlova L. 2011. Fluoroquinolone residues in raw cow’s milk. Czech J Food Sci. 29(6):641–646.

Nirala RK, Anjana K, Mandal KG, Jayachandran C. 2017. Persistence of antibiotic residue in milk under region of Bihar, India. Int J Curr Microbiol App Sci. 6(3):2296-2299.

[OIE] Office Internationale des Epizooties. 2018. OIE list of antimicrobials of veterinary importance [Internet]. [diunduh 2019 Mei 23]. Tersedia pada: https://www.oie.int/fileadmin/Home/eng/Our_scientific_expertise/docs/pdf/AMR/A_OIE_List_antimicrobials_May2018.pdf.

Priyanka, Panigrahi S, Sheoran MS, Ganguly S. 2017. Antibiotic residues in milk a serious public health hazard. J Environ Life Sci. 2(4):99-102.

Raini M. 2016. Antibiotik golongan fluorokuinolon: manfaat dan kerugian. Media Litbangkes. 26(3):163-174.

Sabir AM, Moloy M, Parminder B. 2013. HPLC method development and validation: a review. Int Res J Pharm. 4(4):39-46.

Srinivasu M, Ahmad AH, Kumar N, Pant D, Ahmad W. 2017. Screening of enrofloxacin and its metabolite ciprofloxacin residues by high performance liquid chromatography in cow milk of district Udham Singh Nagar, Uttarakhand. Int J Livest Res. 7(7):140-145.

Thammana M. 2016. A review on high performance liquid chromatography (HPLC). J Pharm Analysis. 5(2):22-28.

Trouchon T, Lefebvre S. 2016. A review of enrofloxacin for veterinary use. J Vet Med. 6:40-58.

Wardyaningrum D. 2011. Tingkat kognisi tentang konsumsi susu pada ibu peternak sapi perah di Lembang Jawa Barat. J Al-Azhar Indon Pra Sos. 1(1):19-26.

Wei Z, Wang J, Zhu L, Wang J, Zhu G. 2018. Toxicity of enrofloxacin, copper and their interactions on soil microbial populations and ammonia-oxidizing archaea and bacteria. Sci Reports. 8(5828):1-9.

DOI: http://dx.doi.org/10.31153/js.v26i1.951