Articles

Found 3 Documents
Search
Journal : Jurnal Ilmu Pertanian Indonesia

Validasi Metode Analisis Kolesterol dalam Telur dengan HPLC-ELSD Lioe, Hanifah Nuryani; Setianingrum, Tika; Anggraeni, Ririn
Jurnal Ilmu Pertanian Indonesia Vol 18, No 3 (2013): Jurnal Ilmu Pertanian Indonesia
Publisher : Institut Pertanian Bogor

Show Abstract | Download Original | Original Source | Check in Google Scholar

Abstract

A method using high-performance liquid chomatography (HPLC) coupled with an evaporative light-scattering detector (ELSD) for the determination of cholesterol in egg was validated. A silica column and a binary mixture of hexane and isopropanol (90:10) as a mobile phase were used to separate cholesterol. Cholesterol was detected at 1.5 min using cholesterol standard and HPLC-ELSD condition: evaporation temperature 50 ºC, air pressure 2.2 bars, and flow rate of mobile phase 2 mL/min. A method linearity for the cholesterol analysis in egg as a sample matrix was obtained at a range of 50 to 3000 µg/g sample, with R2>0.990. Instrument detection limit and limit of quantitation were determined at 1.07 and 3.56 µg/mL, respectively. Recovery test results by spiking cholesterol standard in egg sample at low, medium, and high concentrations (50, 250 and 3000 µg/g ) were 122.13, 108.23, and 44.71%, respectively. Their corresponding repeatability values were 5.26, 4.29, and 10.11%. Method detection limit and intralab reproducibility (to analyze a sample) were observed at 2.30 µg/g and 0.04%. The method is valid for cholesterol analysis in egg at low and medium concentrations. Keywords: cholesterol analysis, egg, HPLC-ELSD, method validation
Validasi Metode Analisis Kolesterol dalam Telur dengan HPLC-ELSD Lioe, Hanifah Nuryani; Setianingrum, Tika; Anggraeni, Ririn
Jurnal Ilmu Pertanian Indonesia Vol 18, No 3 (2013): Jurnal Ilmu Pertanian Indonesia
Publisher : Institut Pertanian Bogor

Show Abstract | Download Original | Original Source | Check in Google Scholar

Abstract

A method using high-performance liquid chomatography (HPLC) coupled with an evaporative light-scattering detector (ELSD) for the determination of cholesterol in egg was validated. A silica column and a binary mixture of hexane and isopropanol (90:10) as a mobile phase were used to separate cholesterol. Cholesterol was detected at 1.5 min using cholesterol standard and HPLC-ELSD condition: evaporation temperature 50 ºC, air pressure 2.2 bars, and flow rate of mobile phase 2 mL/min. A method linearity for the cholesterol analysis in egg as a sample matrix was obtained at a range of 50 to 3000 µg/g sample, with R2>0.990. Instrument detection limit and limit of quantitation were determined at 1.07 and 3.56 µg/mL, respectively. Recovery test results by spiking cholesterol standard in egg sample at low, medium, and high concentrations (50, 250 and 3000 µg/g ) were 122.13, 108.23, and 44.71%, respectively. Their corresponding repeatability values were 5.26, 4.29, and 10.11%. Method detection limit and intralab reproducibility (to analyze a sample) were observed at 2.30 µg/g and 0.04%. The method is valid for cholesterol analysis in egg at low and medium concentrations.
Analisis 3-Monokloro-1,2-Propanadiol (3-MCPD) Ester dalam Minyak Sawit dengan Instrumen Kromatografi Gas-Spektroskopi Massa Lioe, Hanifah Nuryani; Yuliana, Nancy Dewi; Indrasti, Dias; Regiyana, Yane; Putri, Cony Arisya
Jurnal Ilmu Pertanian Indonesia Vol 20, No 2 (2015): Jurnal Ilmu Pertanian Indonesia
Publisher : Institut Pertanian Bogor

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.18343/jipi.20.2.115

Abstract

A group of components called as 3-monochloropropane-1,2-diol (3-MCPD) esters has been found in some vegetable oils, particularly palm oil. Analysis of these components needs GC-MS instrument to reach a low level detection, parts per billion or ppb level. An effort to validate the 3-MCPD esters analysis by GC-MS method (Wei?haar method) using phenyl boronic acid (PBA) as a derivatizing agent and isotopic internal standard (IS) 3-MCPD-D5 followed by the determination of 3-MCPD in commercial palm oils has been conducted. The analytical results showed the instrumental performance as follows: instrument linearity for the analysis of 3-MCPD standard solutions containing IS 2.0 ?g/mL was obtained at a concentration range of 0.25-7.50 ?g/mL test solution with R2 higher than 0.990, precision of 3-MCPD as well as IS retention time was less than 2.0% which was acceptable according to JECFA guidance. Instrument detection limit (LOD) and limit of quantitation (LOQ) were read from GC-MS based on the linearity experiment, i.e. 0.17 and 0.59 ?g/mL solution, respectively. Method linearity by using palm oil as a matrix also showed R2 higher than 0.990. Recovery test result at 40 ?g/g gave an accuracy at 83.29 ± 7.12% which is in the range of AOAC standard (80-110%) and precision at 5.38% (less than RSDHORWITZ). Analysis of 14 palm oils from local market showed 100% of the sampels were positive to contain 3-MCPD esters. 3-MCPD esters in palm oil were found at a concentration range of 8.15-58.14 µg 3-MCPD/g sample.