8/14/2019 Minutes of March 20, 1969 Meeting Rjr-penick

1/5

MINUTES OF MARCH 20, 1969 MEETING

RJR-PENICK & FORD RESEARCH AND DEVELOPMENT PROJECTS

Present : Dr . Murray Senkus

Dr .

Dr .

Mr .

Dr .

R .

R .

W .

E .

E .

E .

C .

C .

Farrar

B r o u i i 1 a r d

Black

Ritchell

Mr . C . M . Sawyer

Dr . P . C . Markunas

Dr . E . D . Nielson

Dr . A . H . Laurene

D r . C . G . Pheil, Jr .V

Dr . Edward Bernasek

I . GLUCOSE-FRUCTOSE

A . Alkaline Isomerization

Laboratory studies on the alkaline isomerization of dextrose have

been initiated to determine if it is possible to produce a glucose-

fructose syrup whi ch has a fructose content of 40 percent or higher .

The th ree approaches currently being investigated are :

1 . Isomerization at ControlledpH

This process is similar to that currently being used in

Cedar Rapids except that the .pH of the isomeri zation mi xture

is maintained constant throughout the reaction . The pH and

temperature ranges being investigated are 7 . 5 - 1 0 .5 and 70-90 C . ,

respectively . Since both dextrose and fructose are rapidly

degraded in concentrated alkaline media, the am ount of alkali

added during the isomerization wi ll be limited to 1% based on~ . . . . . . _ ._ .. _ _ . . . _ . . ..~

dextrose . ,2 Isomerization in Aqueous Alcoholic Medium

.Since our preliminary data indicated a shift in the equilibrium

of the isomerization reaction to higher fructose levels when the

isomerization was carried out in aqueous methanol, it was decided

that a thorough study of this phenomenon should be carried out .

We are currently repeating the isomerizati on in aqueouss methanol

and plan to investigate the isomerization in ethanol and isopropanol .

The amount of alkali being used is 1% based on dextrose .

8/14/2019 Minutes of March 20, 1969 Meeting Rjr-penick

2/5

2

3 . Isomerization Usinq Calcium Hydroxide and Separation

of Fructose and Glucose by Ion Exchange

This process, described by Mr . C . M . Sawyer in CDD- CIM,

1969, No . 1, involves the isomerization of dextrose with

calcium hydroxide by the conventional method and the separation

of fructose from a mixture of glucose, calcium salts of acids

and calcium hydroxide on a Boehringer-type ion exchange column .- - -- -f the ion exchange separation of fructose from the glucose-

-salt- calcium-hydroxide mixture can be performed satisfactorily,

- - - - i t .is conceivable that this process would provide a method for

-- transforming dextrose to fructose in a continuous process .

B . Isomerase

Laboratory studies have demonstrated that a constitutive mutant

can produce glucose isomerase in a medium containing 2% glucose and

no xylose . - - _ ~- --- - -- _ _ _Acute toxicity and antibiotic tests were performed on the parent

strains . This culture w as non-toxic to rats and exhibited no antibiotic

activity . Long-term toxicity tests (30 or 9 0 days), antibiotic assays,

and aflatoxin assays will be performed on the mutant strain .

D r . Nielson stated that if all tests were negative, FDA approval could

probably be obtained within one year .

C . Separation of Glucose and Fructose

1 . B oehringer Process

Preliminary studies .have demonstrated that a calcium form

Boehringer-type ion exchange column can be used to separate

Pensweet syrup into a glucose-rich fraction and a fructose-rich

fraction . It is also possible to obtain a number of fractions

which contain v arying amounts of glucose and fructose . Studies

are being continued to determine the column loading levels and

flow rates w ihich will give optimum separation of glucose and

fructose .

- 2 . Hara .Process

The disclosure on the Hara Process has been receiv ed in_

Winston-Salem and a technical evaluation of the process is

being prepared .

I I . TOTAL SACCHARIFICATION

No commercial a-amylase has been found which has the same type of

activity as the a-amylase in Sumyzyme .

8/14/2019 Minutes of March 20, 1969 Meeting Rjr-penick

3/5

3

Two series of syrups have been run using "run-around" free starch and

"regular" pearl starch . The "run-around" free starch yielded slightly

higher D E syrups . However, the carbohydrate profiles of the final syrups

were similar . In initial studies with Diastase-73, the syrup D E's were

less than those obtained with Nova II . All enzymatic data obtained under

the conditions used in the Komai equipment (pH 5 .0, 600 C .) will be

re-evaluated to determine what additional information is required to further

characterize the commercial glucoamylase enzymes .

The optimal conditions for growth and glucoamylase production by Rhizopus

cultures are under investigation .

Dr . Brouillard will send us a new sample of Sumyzyme .- Dr . Senkus

suggested that acute toxicity and long-term toxicity studies be performed

on Sumyzyme .

I I I . REMOVAL OF DI- AND TRISACC HARIDES FROM TOTAL

SACCHARIFICA ION SYRUP

1 . Granular Carbon

= --- -- - --- - _ - - -- -- - - -- -_ -- -_Laboratory studies have been continued on the evaluation of

the effectiveness of Nuchar C-190 (30 mesh), Pittsburgh activated

(cal 12 x 40) and Darco activated carbon, grade 20 x 40 in sepa-

rating dextrose from the di- and trisaccharides in total sacchar-

ification syrup . Of the three carbons evaluated, the Darco carbon

was the only one which gave a satisfactory separation of the sugars .

The evaluation of the Darco carbon column is continuing to

determine the column loading levels and flow rates which will

give an optimum separation of dextrose and higher saccharides .

~ . Ion Exchange Resins

Preliminary laboratory studies have shown that the potassium

and calcium salts of Dowex 50W cation exchange resins (mesh 100-200 )

giye a sufficiently good separation of dextrose and higher saccharides

to warrant further investigation .

3. Crystallization

It was agreed that no further work should be done on the

-crystallization of dextrose from total saccharification syrup .

IV . BENZYL STARC H

1 . Benzyl Starch-Silica Blend

A three-hundred pound batch of silica treated benzyl starch

has been prepared in our pilot plant and shipped to Owens-Corning

Fiberglass in Aiken, South Carolina .

8/14/2019 Minutes of March 20, 1969 Meeting Rjr-penick

4/5

4

2 . Benzyl Starch-Phosphate Blend

Laboratory studies have demonstrated that the addition of

water soluble phosphates [H3P04, NH4H2PO4 and (NH4)2HP04] to a

30-35% aqueous benzyl starch slurry yields a product which when

ashed gives a residue exhibiting decreased water solubility .

The electrical resistance of the ash obtained from this product

is in the range of 400,000-500,000 ohms . Owens-Corning's

specification for the resistance of an aqueous extract of the

ash remaining on "industrial" grade fiberglass warp after

"burn off" is 100,000 ohms .

Approximately 350 pounds of the benzyl starch-phosphate

blend have been prepared in our pilot plant and shipped to

Owens-Corning Fiberglass plants in Huntingdon, Pennsylvania

and Aiken, South Caroli`na .

V . HIGH LYSINE CORN

Studies carried out in our laboratories and elsewhere have shown that

the protein in high lysine corn is much more soluble in water than the

protein in regular dent corn . We are atternpting to take advantage of this

increased solubility and possibly to enhance it by the use of proteolytic

enzymes which will selectively remove the protein from the starch . It is

our intent to .develop, if possible, a modified separation process which

would operate within the limits of the current steeping process .

Dr . Senkus suggested that Dr . Carey review the high lysine project

at the next meeting .

Twenty-two pounds of high lysine seed corn have been received from

Illinois Foundation Seeds, Inc . and a planting has been made at the

Avoca Farm in Merry Hill, North Carolina .

V I. ELECTROSTATIC SEPARATION OF PROTEIN FROM CORN STARCH

By using a rod electrode charged to 12,000 volts to produce a radial

electrostatic field, it was possible-to achieve a significant difference

in deflection of corn starch and gluten when these materials were caused

to pass through the field area . Quantitative measurements of these

deflections have been obtained and results appear very promising .

Optimization of the geometry and conditions is now in progress .

V I I . PHYSICAL MEASUREMENTS OF SPRAY DRI ED SUCROSE AND TOTAL SUGAR

A report on this work has been circulated .

Porosity tests on samples of PAF 2011 show that of the total volume

of the sugar particle 14% consists of open pores of diameter 0 .5 to 5

microns, 2 .5% consists of open pores of 0 .003 to 0 .03 microns, and 2 to 4%

consists of closed pores of unknown size . Thus, of the total pore volume

in the particle, 80 to 90% is open and available to absorb a substrate and

only 10 to 20% is closed and inaccessible .

8/14/2019 Minutes of March 20, 1969 Meeting Rjr-penick

5/5

- - - - - - - - - - - - - - - - - - - - - - - - S o m e f u r t h e r m e a s u r e m e n t s n o w i n p r o g r e s s o r p l a n n e d a r e p o r o s i m e t e r

and helium pycnometer tests, additional solution rate studies, and tablet-

forming experiments . The tablet-forming tests will be done in cooperation

with the Product Development Department and will include substrate

distribution analysis, porosity analysis, and substrate retention tests .

More effective means of forcing substrate into the sugar particles will

be investigated .

VIII . GRAFTED STARCHES - SCOTT PAPER COMPAPdY

Three samples received February 12, 1969, have been examined and found

to be ineffective as cigarette smoke filtration media . A repo rt on the se

results is in typing .

Edward Bernasek

- E B : j h b

Cc: Dr . C . E . Teague,