Determination of acrylamidein crispbreads by HPLC-MS method

In this study High Performance Liquid Chromatography - Mass Spectrometer ( HPLC-MS) is used to determine the acrylamide content in crispbread which is known as high in starch. However, some parameters such as the type of extraction solvent, solid phase extraction cartridges, injection volumes are modified to get the limit of detection as 4.30 ng/mL and limit of quantitation as 14.30 ng/mL. For the determination of acrylamide in crispbread, liquid chromatograph with mass spectrometer is used with the hareketli phase methanol: 2% aqueous formic acid (80:20) with the flow rate of 0.2ml/min. Extraction process is carried out by using two different methods. One of these methods is the solid phase extraction method in which two different brand of SPE cartridges (Bakerbond and Isolute) are compared. At the end of the study, uncertainty of measurement is calculated for both of the cartridges. The expanded uncertainty of measurement for bakerbond SPE cartridges is calculated as 3.59 and for isolute SPE cartridges it is 0.11.The second method which is used for determination of acrylamide content in crispbread by HPLC-MS is the method known as quechers method which endures the extraction of acrylamide to acetonitril phase from water phase that is salt added to change polarity. It has been remarked that quechers method is not applicable for determination of such low concentrations.At the end of the study, a comparison is made between the two extraction methods and it has been observed that SPE method is more reliable than quechers method. And the comparison that is made between the two SPE cartridges used in SPE method has showen that isolute SPE cartridges give better results than Bakerbond SPE cartridges.The accuracy of the method is proved by the Food Analysis Perfomance Assestment Scheme (FAPAS) obtained from Central Science Laboratory (CSL), York. The acrylamide content of crisp bread which is used fort he validation studies of this study is calculated as 26,17 ±2,9 ng/g crispbread by HPLC-MS method which is implemented by deciding the most appropriate analysis conditions with use of Isolute SPE cartridges.