Determination Of Parabens In Seafoods By Matrix Solid Phase Dispersion Coupled With Gas Chromatography-Mass Spectrometry

Djatmika, Rosalina (2016) Determination Of Parabens In Seafoods By Matrix Solid Phase Dispersion Coupled With Gas Chromatography-Mass Spectrometry. Magister thesis, Universitas Brawijaya.

Abstract

Parabens atau ester dari asam p-hydroxybenzoat digunakan sebagai pengawet antimikroba. Parabens biasanya terdeteksi dalam sistem perairan, termasuk air lingkungan, sedimen dan lumpur. Studi sebelumnya telah melaporkan bahwa paraben memiliki potensi efek jangka panjang pada organisme akuatik dan kesehatan manusia. Parabens menyebabkan gangguan endokrin yang berdampak buruk terhadap sekresi testosteron dan meningkatkan risiko kanker payudara. Metode yang dioptimalkan untuk penentuan paraben dalam makanan laut disajikan. Analye secara bersamaan diekstraksi dan dibersihkan menggunakan prosedur matriks solid-fase dispersi (MSPD). Beberapa kombinasi pelarut elusi, dispersan dan co-sorbent pembersihan diselidiki untuk mendapatkan ekstrak lipid bebas dan pemulihan kuantitatif paraben. Parameter yang mempengaruhi efisiensi ekstraksi MSPD diselidiki oleh desain eksperimental statistik dan analisis varians. Dalam kondisi yang dioptimalkan, 0,5 gram sampel ikan dicampur dengan 0,5 gram natrium sulfat dan tersebar dengan 1,0 gram florisil dan kemudian ditransfer ke kolom SPE yang mengandung 1,5 gram silika: C18 (9: 1) sebagai co-up co-up. Analyte dielusi dengan 12 ml asetonitril. Ekstrak terkonsentrasi pada kekeringan di bawah aliran nitrogen yang lembut dan dibentuk kembali dengan 50 μl metanol. Kemudian, sebagian kecil dari 10 μl dicampur dengan reagen anhidrida asetat 1.0 μL dan langsung disuntikkan ke sistem GC-MS untuk mendapatkan derivatisasi online. Metode yang dioptimalkan menyajikan linearitas yang baik (R2 0,9994) untuk semua analitik target atas konsentrasi tingkat enam dalam berkisar 4-500 ng / g, memberikan batas deteksi rendah kurang dari 0,3 ng / g, diperoleh presisi yang baik (standar deviasi relatif kurang dari 8% Dalam analisis antar dan intra-hari) dan menawarkan pemulihan yang baik (dalam 93% -112%).

English Abstract

Parabens or esters of p-hydroxybenzoic acid are used as antimicrobial preservatives. Parabens are commonly detected in aquatic systems, including environmental water, sediment and sludge. Previous studies have reported that parabens have potential long-term effects on aquatic organisms and human health. Parabens cause endocrine disruptive which adversely affects the secretion of testosterone and enhance the risk of breast cancer. An optimized method for determination of parabens in seafoods was presented. Analytes were simultaneously extracted and cleaned-up using the matrix solid-phase dispersion (MSPD) procedure. Several combinations of elution solvent, dispersants and clean-up co-sorbent were investigated in order to get free-lipid extracts and quantitative recoveries of parabens. The parameters affecting the MSPD extraction efficiency was investigated by statistical experimental design and analysis of variance. Under optimized condition, 0.5 gram of fish sample was mixed with 0.5 gram anhydrous sodium sulfate and dispersed with 1.0 gram of Florisil and then transferred to SPE column containing 1.5 gram of silica:C18 (9:1) as clean-up co-sorbent. Analytes were eluted with 12 mL of acetonitrile. The extract was concentrated to dryness under a gentle stream of nitrogen and re-constituted with 50 μL methanol. Then, a fraction of 10 μL was mixed with 1.0 μL acetic anhydride reagent and directly injected to GC-MS system to obtain online derivatization. The optimized method presented good linearity (R2 0.9994) for all target analytes over six level concentration in ranged 4-500 ng/g, provided low detection limits less than 0.3 ng/g, obtained a good precision (relative standard deviations less than 8% in inter-and intra- day analysis) and offered good recoveries (in ranged 93%-112%).

Item Type:	Thesis (Magister)
Identification Number:	TES/547.038/DJA/d/2016/041611372
Subjects:	500 Natural sciences and mathematics > 547 Organic chemistry
Divisions:	S2/S3 > Magister Matematika, Fakultas MIPA
Depositing User:	Nur Cholis
Date Deposited:	07 Apr 2017 08:58
Last Modified:	17 Jun 2022 07:40
URI:	http://repository.ub.ac.id/id/eprint/157550

Text Thesis-Rosalina Djatmika-2016.pdf Download (3MB)

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