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7   Effects of dam nutrition during pregnancy on gene expression in the late-­‐

7.3   Materials and methods 110

7.3.4   RNA methods 111

7.3.4.1 RNA  extraction  

Cryo-­‐vials  containing  mammary  biopsy  tissue  were  removed  from  -­‐80°C  and  stored   on  dry  ice.  Entire  frozen  biopsy  samples  were  ground  in  300  µl  of  Trizol  reagent  (Invitrogen,   CA,   USA)   with   a   disposable,   sterile   pestle   until   partially   homogenised.   Trizol®   reagent   is   a   mono-­‐phasic  solution  of  phenol  and  guanidine  isothiocyanate  used  to  maintain  the  integrity   of   RNA   while   disrupting   cells   and   dissolving   cellular   components.   Once   partially   homogenised   an   additional   700  µl   of   Trizol®   was   added   and   further   homogenisation   was   performed  with  a  sterile  25  gauge  needle  and  1  ml  syringe.  The  solution  was  left  for  5  mins   at  room  temperature  (RT)  to  allow  complete  dissociation  of  nucleoprotein  complexes,  after   which  200  µl  of  chloroform  was  added  and  mixed  by  vortex  for  15  sec.  The  solution  was  left   to   incubate   at   RT   for   5   mins.   The   samples   were   then   centrifuged   (Thermo   Electron   Corporation   Heracus   pico   17   centrifuge,   Thermo   Fisher   Scientific,   USA)   at   12,000   g   for   15   mins  at  4°C,  to  separate  the  solution  into  aqueous  (RNA-­‐containing)  and  organic  phases.  A   total   of   400  µl   of   the   aqueous   layer   was   removed   and   added   to   an   equal   volume   of   70%  

ethanol  and  mixed  with  the  pipette  tip.  A  Qiagen  RNeasy  kit  (Qiagen,  Netherlands)  was  used   to  further  purify  the  RNA.  RNeasy  kits  are  designed  for  fast  purification  of  high-­‐quality  RNA   using  silica-­‐membrane  RNeasy  spin  columns  which  are  able  to  bind  up  to  100  µg  of  RNA.  A   total   volume   of   700 µl   of   the   RNA-­‐containing   aqueous   solution   and   70%   ethanol   mixture   was  added  to  an  RNeasy  column  which  was  then  centrifuged  at  12,000  g  for  15  sec  to  bind   the  RNA.  The  flow  through  was  discarded.  The  column  was  then  washed  with  350  μl  of  RW1   buffer   using   centrifugation   at   12,000   g   for   15   sec.   This   step   was   repeated   and   the   flow-­‐ through   was   discarded.   A   volume   of   500  µl   of   RPE   buffer   was   added   to   the   column   and   washed  through  using  centrifugation  at  12,000  g  for  15  sec.  Another  500  µl  of  RPE  buffer   was  added  to  the  RNeasy  column  and  centrifuged  for  2  mins  at  12,000  g.  The  column  was   then  placed  in  a  sterile  1.5  ml  eppendorf  and  30  µl  of  diethylpyrocarbonate-­‐  (DEPC)  treated   H20  was  added  to  the  centre  of  the  column  membrane  and  left  to  incubate  for  1  min  at  RT.  

The   samples   were   then   centrifuged   for   1   min   at   10,000   rpm   to   elute   the   RNA   into   a   final   collection   tube.   An   aliquot   was   taken   to   check   the   quantity   and   quality   of   RNA   extracted.   The  remaining  RNA  was  stored  at  -­‐80˚C.  

7.3.4.2 RNA  quantification  

The   concentration   of   RNA   was   determined   using   either   the   NanoDrop   ND-­‐1000   spectrophotometer   (Thermo   Scientific,   MA,   USA)   or   the   Qubit   2.0   fluorometer,   using   the   Qubit  RNA  assay  kit  (Invitrogen).    

The  Nanodrop  measures  the  absorbance  of  an  RNA  or  DNA  sample  at  260  nm  and   provides  the  concentration  in  ng/µl.  The  NanoDrop  also  assess  the  purity  of  each  sample  by   measuring   the   A260   nm/A230   nm   and   A260   nm/A280   nm   ratios.   An   A260:A280   nm   ratio   of  

approximately  2.0  is  generally  accepted  for  pure  RNA.  Pure  DNA  has  a  ratio  of  around  1.8.   Samples  which  have  ratios  below  2.0  may  have  high  levels  of  proteins  or  residual  phenol.   The  A260:A230  nm  ratio  should  be  between  2.0  and  2.2  for  both  RNA  and  DNA.  Ratios  below  

this   suggest   the   presence   of   contaminants   such   as   EDTA,   carbohydrates   or   phenol,   which   absorb   at   230   nm.   Trizol®   reagent   will   absorb   at   both   230   and   270   nm   therefore   any   remaining  Trizol  reagent  will  affect  these  ratios.    

The   Qubit   uses   fluorescent   dyes   to   quantify   biomolecules   of   interest.   The   fluorescent  dyes  only  emit  a  signal  when  they  are  bound  to  specific  target  molecules  (e.g.,   RNA).   The   Qubit   has   an   advantage   over   the   Nanodrop   in   that   the   fluorescent   dyes   are   specific   to   the   type   of   molecule   being   measured   (Bustin  et   al.,   2009).   Therefore,   even   if   there  is  DNA  present  in  a  sample,  only  the  concentration  of  RNA  will  be  given.    

7.3.4.3 RNA  agarose  gels  

The  integrity  of  total  RNA  in  samples  was  checked  by  running  a  small  volume  on  a   1%  agarose  gel  for  quality  control.  Agarose  gels  were  made  with  sodium  boric  acid  buffer  to   which   50   μl   of   10   mg/ml   ethidium   bromide   stock   solution   was   added   giving   a   final   concentration  of  0.5  µg/ml.  Approximately  1  µl  of  loading  dye  (25%  bromophenol  blue  (1%   solution),  25%  xylene  cyanol  (1%  solution),  30%  glycerol  and  20%  MilliQ  H20)  was  added  to  

each   sample,   then   10  µl   of   each   sample   was   loaded   on   to   the   gel.   A   DNA   ladder   (1   kb+,  

Invitrogen)  was  also  loaded  to  one  lane  as  a  marker  to  determine  the  size  of  bands  and  as  a   control  to  check  the  quality  of  the  gel.  Gels  were  run  for  10  to  20  mins  at  2000  V  (as  RNA   begins  to  degrade  if  run  for  longer  periods).  Gels  were  run  with  Owl  B1A  EasyCast  Mini  Gel   systems  (Thermo  Scientific)  using  an  EC250-­‐90  power  supply  (Thermo  Scientific).  Gels  were   viewed   under   ultraviolet   light   and   RNA   checked   for   degradation.   Intact   total   RNA   should   have   sharp   28S   and   18S   rRNA   bands;   the   28S   band   should   be   approximately   twice   the   intensity  of  the  18S  band  (indicating  a  2:1  ratio).  If  RNA  is  partially  degraded,  the  rRNA  bands   will  be  smeared  in  appearance,  rather  than  sharp,  or  will  not  have  the  2:1  ratio.  Completely   degraded  RNA  will  appear  as  a  low-­‐molecular-­‐weight  smear.    

7.3.4.4 RNA  pools  

The  findings  of  Martin  et  al.  (2012)  and  those  reported  in  Chapter  5  demonstrated   that   dam   nutrition   during   early   pregnancy,   as   opposed   to   mid-­‐to-­‐late   pregnancy,   affected   mammary   gland   development   and   first-­‐lactation   performance   of   offspring   (Paten  et   al.,   2013).  Therefore,  in  the  present  study,  only  samples  from  ewes  born  to  dams  which  were   differentially  fed  during  early  pregnancy  and  fed  maintenance  during  mid-­‐to-­‐late  pregnancy   (SmM,  MM  and  AdM)  were  used  for  transcriptome  analysis.  For  RNA-­‐sequencing,  RNA  from   multiple  individuals  within  a  treatment  and  time  point  was  pooled  in  an  attempt  to  minimise   variation   among   samples   (Kendziorski  et   al.,   2003;   Kendziorski  et   al.,   2005;   Konczal  et   al.,   2014).  Approximately  2  µg  of  RNA,  subsampled  from  three  randomly  selected  animals  per   treatment,   was   incorporated   into   pools.   Three   pools   per   treatment   were   generated   for   samples   taken   during   late   pregnancy   and   two   pools   were   generated   per   treatment   for   samples  taken  during  lactation,  due  to  the  reduced  number  of  lactation  samples.  The  pools   were:  late  pregnancy;  SmM,  MM,  and  AdM  (n  =  3  pools  sequenced  for  each  treatment,  with   three  samples  per  pool,  n  =  9  total  samples  for  each  treatment),  and  lactation;  SmM,  MM,   and  AdM  (n  =  2  pools  sequenced  for  each  treatment,  with  three  samples  per  pool,  n  =  6  total   samples  per  treatment).  Therefore,  the  number  of  pools  used  to  examine  gene  expression  in   late   pregnancy   versus   lactation   (irrespective   of   treatment)   was   as   follows:  n  =   9   pools   for  

late  pregnancy,  with  three  samples  per  pool,  n  =  27  samples;  and  n  =  6  pools  for  lactation,   with  three  samples  per  pool,  n  =  18  samples.  A  diagram  of  the  pooling  strategy  can  be  found   in  Chapter  8  (Figure  8.1).    

7.3.4.5 Bioanalyzer  

The  quality  of  pooled  RNA  samples  was  checked  using  the  Agilent  2100  Bioanalyzer   with   the   Agilent   RNA   6000   pico   chip   (Agilent   Technologies,   CA,   USA).   The   bioanalyzer   is   a   microfluidics-­‐based   system   which   utilises   capillary   electrophoresis   to   separate   RNA   molecules   based   on   size.   The   RNA   chip   contains   wells   in   which   the   samples   are   loaded.   Micro-­‐channels  fabricated  in  glass  create  interconnected  networks  among  the  wells  in  the   chip.  When  the  chip  is  prepared,  the  micro-­‐channels  are  filled  with  a  fluorescence-­‐gel-­‐dye   mix.  Once  the  wells  and  channels  are  filled,  the  chip  becomes  an  integrated  electrical  circuit.   When  the  chip  is  placed  in  the  bioanalyzer,  a  16-­‐pin  electrode  fits  into  the  wells  of  the  chip   and  charged  biomolecules  (e.g.,  RNA)  are  electrophoretically  driven  by  a  voltage  gradient.   Because   of   a   constant   mass-­‐to-­‐charge   ratio   and   the   sieve-­‐like   activity   of   the   gel,   the   molecules  are  separated  by  size,  with  smaller  fragments  migrating  faster  than  larger  ones.   Dye  molecules  complex  with  RNA  strands  and  are  detected  by  laser-­‐induced  fluorescence.   Data   is   then   translated   into   gel-­‐like   images   (with   bands)   and   electropherograms   (peaks),   which  are  interpreted  much  like  a  conventional  gel  electrophoresis  (i.e.,  Intact  samples  have   a   28S   and   18S   rRNA   bands   with   a   2:1   ratio).   The   RNA   integrity   number   (RIN)   is   derived   through   the   bioanalyzer   software   and   determines   the   amount   of   degradation   present   in   each  sample  (Schroeder  et  al.,  2006).  A  RIN  of  seven  or  greater  (RIN  ranges  from  1,  totally   degraded,   to   10,   intact)   is   deemed   acceptable   for   sequencing   as   it   indicates   little   degradation.