Determination of Morpholine Fatty Acid Salt Residues in Fruits by Improved QuEChERS-Gas Chromatography- Tandem Mass Spectrometry
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Abstract:
In this study, a gas chromatography-tandem mass (GC-MS/MS) method was developed to determine the morpholine fatty acid salt in fruits. Samples were analyzed using a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) method, through being extracted with 1% formic acid-acetonitrile, purified with ethylenediamine-N-propylsilane (PSA) and graphitized carbon black adsorbent (GCB), derivatized with 5.5 mol/L HCl and 4.3 mol/L NaNO2 in ice bath for 3 h, separated by HP-FFAP capillary column, and measured in electron bombardment ion source (EI) and multiple reaction monitoring mode. Matrix calibration curve and external standard method were used for quantification. The results showed that morpholine fatty acid salts can be derivatized into stable nitrosomorpholine (NMOR) through nitrosation. The peak shape of the target derivative compound was good, The linearity in the analyte range of 1~800 µg/L was good, with the correlation coefficient higher than 0.99, the limit of detection as 0.14~1.09 µg/kg, the limit of quantitation as 0.47~3.63 µg/kg, the recovery rate of spiked standard as 73.6%~118.5%, and the relative standard deviation (RSD) as 3.6%~15.2% (n=6). This method is accurate and efficient, has a high detection rate in actual samples, and is suitable for qualitative and quantitative detection of morpholine fatty acid salt in fruits.