Quantification of FAMEs in biodiesel blends of various sources by gas chromatography tandem mass spectrometry

2015 ◽  
Vol 7 (8) ◽  
pp. 3372-3378 ◽  
Author(s):  
Syed Ghulam Musharraf ◽  
Muhammad Arif Ahmed ◽  
Noureen Zehra

A quantification method for FAMEs by GC-MS/MS in multiple reaction monitoring (MRM) mode was developed and validated in the various biodiesels and their blends.

Author(s):  
Bianey Garcia Lara ◽  
Israel Enciso Donis ◽  
Katarzyna Wrobel ◽  
Kazimierz Wrobel

<p>The term “phthalates” refers to a group of esters of benzene-1,2-dicarboxylic acid, widely used as plasticizers therefore ubiquitous in food and in the environment. Several phthalates have been cataloged as endocrine disruptors and that is why there is a strong demand for their reliable determination, especially in food matrices.  In the present work, gas chromatography - tandem mass spectrometry (GC-MS/MS) procedure is proposed for the determination of six priority phthalates (dimethyl phthalate DMP, diethyl phthalate DEP, di(n-butyl) phthalate DBP, benzyl butyl phthalate BBP, di(2-ethylhexyl) phthalate DEHP, di(n-octyl) phthalate DnOP) and di(2-ethylhexyl) adipate DEHA, in maize tortillas and flour. Fresh tortilla sample was homogenized with acetonitrile/water (1:1) and after salting out (NaCl), hexane extract was obtained and dried by addition of Na<sub>2</sub>SO<sub>4</sub> anhydride. Finally, solvent was evaporated and the residue was reconstituted in isooctane for the injection to GC-MS/MS system; a model SCION GC-TQMS from Bruker Daltonics was used for the analysis. Quantification was carried out by multiple reaction monitoring (MRM) with the following time segments and m/z values of the precursor/product ion transitions: 0-7.90 min, 163/133 DMP; 7.47-8.53min, 149/121 DEP; 8.53-9.93 min, 149/121 DBP; 9.93-12.39 min, 149/93 BBP; 11.40-12.44 min, 129/111 DEHA; 12.20-13.22 min, 149/121 DEHP; 13.13-14.20 min, 149/121 DnOP. The evaluated method detection limits for seven compounds were in the range 0.11-1.84 µg kg<sup>-1</sup> (tortilla dry mass). The results obtained for fifteen tortilla samples purchased in Guanajuato state were as follows: 71.6-420 µg kg<sup>-1</sup> DEHP &gt; not detected (nd)-274 µg kg<sup>-1</sup> DBP &gt; nd-197 µg kg<sup>-1</sup> DEHA &gt; nd-73.2 µg kg<sup>-1</sup> DEP &gt; nd-10.6 µg kg<sup>-1</sup> DnOP. It was observed that prolonged storage and elevated temperature favored the accumulation of phthalates in tortillas.</p>


1990 ◽  
Vol 73 (6) ◽  
pp. 973-980 ◽  
Author(s):  
Javier Plasencia ◽  
Chester J Mirocha ◽  
Robert J Pawlosky ◽  
John F Smith

Abstract The present paper describes a sensitive procedure for quantitative analysis of the Fusarlum mycotoxins zearalenone and α-zearalenol in urine of ruminants. Extraction is done with an octadecyl (C18) column and cleanup with a silica column providing a preparation that Is analyzed by gas chromatography- tandem mass spectrometry (GC-MS/MS). The trlmethylsllyl ether derivatives of zearalenone and a-zearalenol yield molecular ions with m/z 462 and 536, respectively. These Ions are selected In the first mass analyzer and then fragmented In a collision cell to give characteristic daughter Ions (m/z 151, 333, 318, and 446). The method is known as multiple reaction monitoring (MRM). Elimination of chemical background noise by selecting proper fragment ions produces chromatograms in which Identification and quantitation in a biological matrix is possible. The method was tested with sheep urine from an experimental feeding trial and was used to confirm natural mycotoxlcosis of cows affected with zearalenone. Zearalenone (1 ppb) and a-zearalenol (14 ppb) were found In 2 different cow urine samples. The detection limit for both zearalenone and zearalenol Is 1 ppb (1 ng/mL) In urine and Is linear between 1 and 20 ppb for the former and 1 and 10 ppb for the latter.


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