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Simultaneous Determination of 13-HODE, 9,10-DHODE, 9,10-EPODE and 9,10,13-THOD in Cured Meat Products by HPLC-MS/MS

SONG Hui, GENG Zhiming, REN Shuang, WANG Daoying, ZHANG Muhan, SUN Chong, XU Weimin   

  1. 1.Key Laboratory of Meat Processing and Quality Control, Ministry of Education, Nanjing Agricultural University, Nanjing
    210095, China; 2. Institute of Agricultural Products Processing, Jiangsu Academy of Agricultural Sciences, Nanjing 210014, China;
    3. Collaborative Innovation Center of Meat Production and Processing, Nanjing 210095, China
  • Online:2016-09-25 Published:2016-09-26
  • Contact: XU Weimin

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Abstract:

13-Hydroxy-9,11-octadecadienoic acid (13-HODE), 9,10-dihydroxy-12-octadecenoic acid (9,10-DHODE),
9,10-epoxyoctadec-12-enoic acid (9,10-EPODE) and 9,10,13-trihydroxy-11-octadecenoic acid (9,10,13-THODE) in cured
meat products were detected with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).
The analytes, extracted with methanol and cleaned by solid phase extraction, were separated on an XBridge C18 column with
a mobile phase consisting of 0.1% formic acid in water and acetonitrile, followed by ionization and quantification with an
electrospray ionization source in negative ion mode and multiple reaction monitoring mode (MRM). The results indicated
that the calibration curves for 13-HODE, 9,10-DHODE, 9,10-EPODE and 9,10,13-THODE exhibited good linearity
(R2 > 0.999) in the ranges of 0.05–2.0, 0.01–0.5, 0.05–1.0 and 0.01–0.5 μg/mL, respectively. The limits of detection (LODs)
for the four analytes were 0.120, 0.008, 0.200, and 0.016 μg/g, and the recoveries were 95.1%, 85.2%, 86.8% and 86.2%,
respectively. The method was successfully employed to detect the analytes in 26 cured meat products and the results
showed that all the samples contained 13-HODE, 9,10-DHODE and 9,10,13-THODE ranging from 1.4–100.7, 0.1–3.9 and
0.4–10.2 μg/g, respectively, and out of these samples, 21 contained 9,10-EPODE ranging from 0.8–6.9 μg/g. Since some
isomers of the analytes were detected in samples as well, the real content of fatty acids with hydroxyl group (s) from
oxidation of linoleic acid (LA) might be much higher.

Key words: linoneic acid, cured meat products, 13-HODE, 9,10-DHODE, 9,10-EPODE, 9,10,13-THODE, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)

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