The 3-monochloropropane-1,2-diol (3-MCPD) and 3-MCPD esters were found in any type of refined vegetable oil -mostly produced during the refining process-and recognized as emerging food contaminants. Several analytical methods have been developed and one of which was a Weißhaar's method. The study aims to validate the modified Weißhaar's method for analysis of 3-MCPD and 3-MCPD esters in refined palm oil. Ion fragments were used for identification and quantification of 3-MCPD and 3-MCPD-d5. 3-MCPD was determined by GC-MS after released from its ester by transesterification with sodium methoxide and derivatized with phenylboronic acid. The validation showed that liniarity response (r=0.994) was observed from a linear regression by using external standard and internal standard at a concentration range of 0.008 and 0.377 µg mL -1 . The LOD of the validated method was 0.06 µg g -1 while its LOQ was 0.20 µg g -1 , precision (relative standard deviation, RSD) was 6.16%, and accuracy (as percentage of recovery) was in the range of 95.83-113.27%. This results indicated that the modified method was valuable and sensitive for detection of 3-MCPD and 3-MCPD esters. Using the validated method, 3-MCPD esters content of a commercial palm oil sample was determined and calculated as the difference between total 3-MCPD and free 3-MCPD, which was 13.24 µg g -1 . Total 3-MCPD content of several palm oils were at a concentration range of 13.94-34.52 µg g -1 . These results also showed that there was a correlation between 3-MCPD with diacylglyceride (DAG). Samples with DAG content gave a high test results of 3-MCPD with a coefficient of correlation of r=0.752.
ABSTRAKSenyawa 3-monochloropropane-1,2-diol (3-MCPD) dan esternya merupakan kontaminan yang umumnya terbentuk pada proses pengolahan pangan. Kontaminan ini termasuk food emerging yang berpotensi mempengaruhi kesehatan manusia. Beberapa metode analisis telah dikembangkan untuk penetapan kadar 3-MCPD dan esternya dan salah satunya adalah metode Weißhaar yang digunakan untuk menguji minyak safflower. Penelitian ini bertujuan untuk memvalidasi metode analisis Weißhaar yang dimodifikasi dan metode ini digunakan untuk minyak goreng sawit. 3-MCPD ester dibebaskan dari esternya oleh natrium metoksida secara transesterifikasi kemudian 3-MCPD bebas diderivatisasi dengan phenylboronic acid dan diidentifikasi secara GC-MS dengan menggunakan fragmen ion. Validasi metode analisis yang dilakukan memberikan hasil sebagai berikut: dari persamaan regresi y= 0.076x + 0.005, y adalah rasio area baku pembanding eksternal dan internal, x adalah konsentrasi baku pembanding eksternal, didapatkan linearitas yang ditunjukkan oleh koefesien korelasi (r) 0.994 pada rentang kerja 0.008-0.377 µg mL -1 ; batas deteksi pada 0.06 µg g -1 , batas kuantitasi pada 0.20 µg g -1 ; presisi dinyatakan sebagai koefisien variasi sebesar 5.89%; akurasi dihitung sebagai persen rekoveri dengan nilai 95.83-113.27%. Hasil validasi metode analisis ini memenuhi kriteria yang telah dipersyaratkan. Kadar 3-MCPD ester dihitung se...