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PDF - White Rose Etheses Online

PDF - White Rose Etheses Online

PDF - White Rose Etheses

Development of an LC-MS/MS method for the analysis of triacylglycerols from meat and application in the discrimination of cooked meat products HASLINA HASAN A thesis submitted in partial fulfilment of the requirement for the degree of Doctor of Philosophy at the University of York Department of Chemistry University of York June 2010

  • Page 2 and 3: Abstract A single stage reversed ph
  • Page 4 and 5: 1.8 Chapter 2 2.1 2.2 1.7.3 Mass sp
  • Page 6 and 7: 3.3 Chapter 4 4.1 4.2 4.3 Chapter 5
  • Page 8 and 9: LIST OF TABLES Chapter 1 Table 1.1
  • Page 10 and 11: 6.4 6.5 LIST OF FIGURES Chapter 1 F
  • Page 12 and 13: 2.16 2.17 2.18 2.19 2.20 2.21 2.22
  • Page 14 and 15: 3.5 3.6 3.7 3.8 3.9 3.10 3.11 3.12
  • Page 16 and 17: 4.12 4.13 4.14 4.15 4.16 4.17 4.18
  • Page 18 and 19: ITMS ion trap mass spectrometry L l
  • Page 20 and 21: AUTHOR’S DECLARATION I hereby dec
  • Page 22 and 23: 1.1 Food authenticity and adulterat
  • Page 24 and 25: of adulteration, namely scanning el
  • Page 26 and 27: 1.3 Nomenclature and structures of
  • Page 28 and 29: Table 1.1: Scientific names, chemic
  • Page 30 and 31: Table 1.2: Abbreviations, trivial n
  • Page 32 and 33: The ECL (equivalent chain length) o
  • Page 34 and 35: 1.5.2.2 Separation of positional is
  • Page 36 and 37: 1.7 Background on instrumentation 1
  • Page 38 and 39: technique was named ultra high perf
  • Page 40 and 41: The series of reactions occurring i
  • Page 42 and 43: 1.7.3.3 Ion trap mass spectrometry
  • Page 44 and 45: az 0.4 r stability z stability 0.2
  • Page 46 and 47: 1.8 Aims of the research The overal
  • Page 48 and 49: 2.1 Introduction and aims Introduct
  • Page 50 and 51: POP-PPO and PLP-PPL was demonstrate
  • Page 52 and 53:

    a) 100 Relative abundance b) 0 100

  • Page 54 and 55:

    a) b) 100 Relative abundance 100 Re

  • Page 56 and 57:

    In the absence of ammonium acetate

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    a) b) Relative abundance 100 Relati

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    a) 100 Relative Abundance b) Relati

  • Page 62 and 63:

    2.2.3 Development of a single stage

  • Page 64 and 65:

    was observed in both columns, showi

  • Page 66 and 67:

    a) Relative Abundance b) Relative A

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    ECN (45, 47, 49, 51 and 53) were ob

  • Page 70 and 71:

    The replacement of 2-propanol by ch

  • Page 72 and 73:

    Relative Abundance peaks are still

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    The chromatogram from the Waters Sp

  • Page 76 and 77:

    Relative Abundance Relative Abundan

  • Page 78 and 79:

    Relative Abundance a) b) 100 0 Abun

  • Page 80 and 81:

    Relative Abundance a) 100 b) 100 Re

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    The region of the spectrum in which

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    2.2.3.3 CID of ammoniated TAG ions

  • Page 86 and 87:

    ABA and AAB TAGs Symmetric and asym

  • Page 88 and 89:

    The MS and MS 2 chromatograms for b

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    ABC TAGs ABC type TAGs contain 3 di

  • Page 92 and 93:

    a) Relative Abundance b) c) d) 100

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    Table 2.7: TAG identifications from

  • Page 96 and 97:

    2.2.3.4 CID of DAG product ions in

  • Page 98 and 99:

    Relative Abundance a) b) Relative A

  • Page 100 and 101:

    The major TAGs with an ECN value of

  • Page 102 and 103:

    this study. It started with a very

  • Page 104 and 105:

    Relative Abundance Figure 2.24: RP

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    Relative Abundance 2.2.4.2 Mass spe

  • Page 108 and 109:

    Relative Abundance For the POP/PPO*

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    Within the SOP*/SPO* isomer group (

  • Page 112 and 113:

    Relative Abundance For the isomer p

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    Relative Abundance In the SLO*/SOL*

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    Table 2.9: Percentages of TAG isome

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    Chicken has similar TAG isomer abun

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    The chromatogram of TAGs produced f

  • Page 122 and 123:

    2.3 Conclusions The dissociation be

  • Page 124 and 125:

    CHAPTER 3 FA and TAG variations in

  • Page 126 and 127:

    (Huerta-Leidenz et al., 1996). Sign

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    Relative abundance a) Lamb b) Beef

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    chicken and beef have similar propo

  • Page 132 and 133:

    3.2.2 FA profiles from different an

  • Page 134 and 135:

    contains more saturated FAs than SC

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    a) b) % of FAMEs % of FAMEs 60 50 4

  • Page 138 and 139:

    The PUFA contents show considerably

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    The individual TAG peak areas of al

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    % of TAGs 35 30 25 20 15 10 5 0 LLL

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    a) b) % of TAGs c) % of TAGs d) % o

  • Page 146 and 147:

    Relative abundance 3.2.4 TAG profil

  • Page 148 and 149:

    al., 2004 and Viera Alcaida et al.,

  • Page 150 and 151:

    a) % of TAGs b) % of TAGs 30 25 20

  • Page 152 and 153:

    Figure 3.13: PCA scores plot of FAM

  • Page 154 and 155:

    3.2.5.2 PCA of TAGs for beef, lamb,

  • Page 156 and 157:

    a) b) Loadings values c) Loadings v

  • Page 158 and 159:

    Improved separation of TAGs in this

  • Page 160 and 161:

    Figure 3.17: PCA scores plot of FAM

  • Page 162 and 163:

    3.2.6.2 PCA of TAGs of adipose tiss

  • Page 164 and 165:

    Analysing the variation in the TAG

  • Page 166 and 167:

    (LPS). Comparison between SC fat fr

  • Page 168 and 169:

    CHAPTER 4 Analysis of TAGs for disc

  • Page 170 and 171:

    samples. Although there were some m

  • Page 172 and 173:

    4.2 Results and discussion The thre

  • Page 174 and 175:

    Figure 4.1: Chromatograms of TAGs f

  • Page 176 and 177:

    Chapter 4: Analysis of TAGs for dis

  • Page 178 and 179:

    with the saturated FA in the sn-2 p

  • Page 180 and 181:

    The histogram of raw beef, curry (i

  • Page 182 and 183:

    The histograms for raw and cooked l

  • Page 184 and 185:

    The TAG profiles for different meth

  • Page 186 and 187:

    Table 4.4: Reassessed proportions o

  • Page 188 and 189:

    The TAG proportions for raw pork we

  • Page 190 and 191:

    4.2.4 PCA of TAG profiles for raw a

  • Page 192 and 193:

    The PCA scores plot for the TAG pro

  • Page 194 and 195:

    a) b) c) Loadings value Loadings va

  • Page 196 and 197:

    a) b) Loadings value c) Loadings va

  • Page 198 and 199:

    4.2.4.4 PCA of TAGs for raw and coo

  • Page 200 and 201:

    4.2.5 PCA of TAG profiles for raw a

  • Page 202 and 203:

    Table 4.5: The reassessed proportio

  • Page 204 and 205:

    PC2 shows the variation between cla

  • Page 206 and 207:

    The loadings values of PC1 and PC2

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    Since added TAGs were also observed

  • Page 210 and 211:

    4.3 Conclusions Microwave cooking o

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    CHAPTER 5 Overall conclusions and f

  • Page 214 and 215:

    fats show good potential for discri

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    differentiation between animal spec

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    5.2 Future work. Aspects of this re

  • Page 220 and 221:

    CHAPTER 6 Experimental

  • Page 222 and 223:

    a) b) Loin Ham Belly Shoulder Figur

  • Page 224 and 225:

    6.1.3 Extraction procedure 6.1.3.1

  • Page 226 and 227:

    6.1.4 Hydrolysis and methylation of

  • Page 228 and 229:

    The GC gradient programme used for

  • Page 230 and 231:

    6.2.3 RSLC-HCT Ultra high performan

  • Page 232 and 233:

    References

  • Page 234 and 235:

    Bligh E.G., Dyer W.J., A rapid meth

  • Page 236 and 237:

    De Boer J., Chlorobiphenyls in boun

  • Page 238 and 239:

    Franco I., Escamilla M.C., Garcia J

  • Page 240 and 241:

    Hvattum E., Analysis of triacylglyc

  • Page 242 and 243:

    Leskinen H., Suomela J.P., Kallio H

  • Page 244 and 245:

    Momchilova S., Nikolova-Damyanova B

  • Page 246 and 247:

    Rezanka T., Sigler K., The use of a

  • Page 248 and 249:

    Tsimidou M., Macrae R., Reversed-ph

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