1/29/97


I am also interested in staining for calcium. My subject is Douglas Fir

ectomycorrhizal with a basidiomycete fungus, Rhizopogon vinicolor. I am

trying to localize calcium in the fungal tissue and in the interface area

between the plant and the fungal cells. Tracers for calcium have proven

difficult, i.e. flourescent probes for calcium do not cross fungal

membranes and are probably too large to pass through cell walls as calcium

does. I am interested in references on Alizarin red, or "Dahl's method for

Calcium", whether these are applicable to botanical specimens, and what

about fixing the calcium in place so that it is not displaced by

sectioning, etc., prior to staining? Thanks in advance for any advice.

Janet K. Dye

Ph. D. Graduate Student, Soils

Land, Air, and Water Resources

University of California

Davis, California USA

(916) 752-0199

(916) 668-4217

jkdye@ucdavis.edu


Especially to Janet Dye and Linda fox

The Alizarin technique for calcium is called "Dawsons" and is quite old. We

don't have the original reference, but for bone the proceedure is: fix in

10% NFS, wash then transfer to 0.5% aq KOH to which enough alizarin red S

has been added to turn solution to deep purple, leave for 24 hours or till

bones are distinctly red, transfer thro KOH-glycerine series,3:1, 1:1, 1:3,

to pure glycerine. Store in pure glycerine plus few crystals of thymol.

Refs for meth blue plus alizarin red staining of bone may help: Bechtol

1948 Stain Technol 23, p3-9; Burdi and Flecker 1968 Stain Technol 43,

p47-48; Lundvall 1927 Anat Anz 62, p353-373. If you still require more

info, contact me via e-mail and we will try to help.

Miss A.J.Wilson

Electron Microscope Unit

St George's Hospital Medical School

Cranmer Terrace

Tooting London SW17 ORE

Tel: 0181 725 5220


We found Dawson's original technique for alizarin preparations:

1. Fix in 95% ALC for 48-72Hrs. Prolonged fix in alcohol renders tissue

less liable to maceration.

2. Remove fats in acetone for 2-4 days then return specimens to alcohol for

12-24 hrs.

3. Place in 1% KOH until bones or digits appear thro' muscle

Transfer to 0.1% Alizarin Red S in 1% KOH. (Other stains eg alcian blue, or

victoria blue can be used to counter-stain cartilage or bone at this

stage.)

4. Leave till stained or desired bone colour, change to fresh stain if

necessary.

5. CLEARING

Place in solution of 1g KOH, 20mls glycerine, 79mls dist water, leave till

sample clears.

6. When clear, pass thro' increasing conc of glycerine, 50, 70, 90, 100%

Miss A.J.Wilson

Electron Microscope Unit

St George's Hospital Medical School

Cranmer Terrace

Tooting London SW17 ORE

Tel: 0181 725 5220

awilson@s1.sghms.ac.uk


Thanks to Amanda Wilson, Bruce Wagner, and David Brauer for recommendations

and comments.

Bruce has recommended (pyro?) antimonate to precipitate Ca in place,

localizing it, and I assume followed by TEM and electron probe to confirm

the presence of Ca. I have heard of this technique, especially as applied

to plants which employ sequestering of excess Ca as oxalate crystals in

specialized cells called idioblasts. But I have also heard that your

specimen must have very high levels of Ca present in some form, such as Ca

crystals, in order for this method to work. So I also would assume that

this method won't work for Ca which is held on the ion exchange groups of

the cell wall, or as non-crystalline co-ions in the vacuole?

Anyway, I will read up on the pyroantimonate method and see if it will

track Ca even when it isn't a precipitate. Also will look at Alizarin red

and try to translate to botanicals.

Thanks, Janet.

Janet K. Dye

Ph. D. Graduate Student, Soils

Land, Air, and Water Resources

University of California

Davis, California USA

(916) 752-0199

(916) 668-4217

jkdye@ucdavis.edu


Dear Janet,

> Bruce has recommended (pyro?) antimonate to precipitate Ca in place,

Yes, pyroantimonate. This can, however, wreck havoc with the

ultrastructure; try it and see.

> localizing it, and I assume followed by TEM and electron probe to confirm

> the presence of Ca.

You can also locate the antimony by EDS.

> I have heard of this technique, especially as applied

> to plants which employ sequestering of excess Ca as oxalate crystals in

> specialized cells called idioblasts.

If you have ~ micron-sized CaC2O4 xtals, you can use EDS directly

without using pyroantimonate--there is plenty of Ca in them.

> But I have also heard that your

> specimen must have very high levels of Ca present in some form, such as Ca

> crystals, in order for this method to work. So I also would assume that

> this method won't work for Ca which is held on the ion exchange groups of

> the cell wall, or as non-crystalline co-ions in the vacuole?

EDS needs a large fraction of a %, or ~mM concentrations (wet) to

detect and quantitate an element. It is irrelevant what the chemical form

of the element is. These amounts must only be present in the analysed

volume; the overall amount can be very much less as long as it is present

in small, concentrated regions.

> Anyway, I will read up on the pyroantimonate method and see if it will

> track Ca even when it isn't a precipitate.

Any Ca++, and other Ca which has a greater affinity for pyroan-

timonate than for its ligands will be precipitated. Good luck.

Yours,

Bill Tivol

tivol@wadsworth.org


The detection limit of averaged (or, when feasible, high dose) Ca

measurements with EPMA (=EDS) is about 0.3 mmole/kg dry wt.

Dr. Andrew P. Somlyo

aps2n@elvis.med.virginia.edu


Janet,

Charley Smalls and I used the pyroantinomate method years ago to localize Ca2+

in developing muscle at sites where Ca2+ is not normally crystaline. However,

it also precipitates Mg2+ if I recall, so you have to do some special

controls. The refs are in our paper:

Smalls, C.M. & Goode,D. (1977) Ca+2 - accumulating components in

developing skeletal muscle. J. Morphol.151: 213-238.

Dr. M. Dennis Goode Phone (301) 405-6917

Department of Zoology Fax (301) 314-9358

University of Maryland e-mail goode@zool.umd.edu

College Park MD 20742


Bill Tivol, Dr. Somlyo, and Dennis Goode, Thank you for the advice. The

detection limit for Ca by EPMA=EDS, or electron probe, is suprisingly high.

My results with the fungus I work with would indicate a 100 x higher level

of Ca held in exchangeable form on the cell walls, after exposure to

realistic soil solution levels of Ca. And the literature on the host

plant, Douglas Fir, would indicate Ca levels 25-30 x higher than the fungus

(making some assumptions there). So, apparently, electron probe will do

this, although I understand that asking a yes/no tracer question is a lot

easier than asking how much Ca (and how exact?). Ca oxalate crystals have

been observed to form in the walls and possibly in the vacuoles/vesicles of

the structure I work with, so confirming that is not very interesting.

What is interesting is where did the Ca come from is such quantities and

where does it go, if anywhere. (The normal habitat for this symbiosis is

an acidic, leached, relatively low Ca soil.) Maybe using Sr (stable) as a

short term tracer for Ca is more useful. Still reading up and thinking,

Janet.

Janet K. Dye

Ph. D. Graduate Student, Soils

Land, Air, and Water Resources

University of California

Davis, California USA

(916) 752-0199

(916) 668-4217

jkdye@ucdavis.edu


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