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Statement of
Compliance -------------------------------------------- 2
Quality Assurance
Statement----------------------------------------- 3
Signature of Approval
---------------------------------------------- 5
I ) Summary
--------------------------------------------------------12
II) Purpose
--------------------------------------------------------16
A.
General ----------------------------------------------------16
B.
Protocol amendments ----------------------------------------17
1.
Processing experiment(#1): add line 40-3-2 ----------17
2.
Processing experiment(#2): full-fat soybean flour
was prepared---------------------------------------17
3. Processing
experiment(#3): toasted meal samples
were
retoasted ------------------------------------17
4.
Analytical experiment (#1) : add line 40-3-2 ---------17
5. Analytical experiment (#2) : the retoasted meal
was substituted for the initially-toasted meal
for the analytical assays -------------------------17
6. Analytical experiment (#3) : the enzymatic activity
of CP4 EPSPS and GUS were determined in pooled
seed extracts -------------------------------------17
7.
Analytical experiment(#4) : one set of six seeds
from each plot was used for the ELISA expression
analysis, not two sets ----------------------------17
8. Analytical experiment(#5) : ELISA assays were
performed on the seed pool extracts analyzed
by functional enzymatic assay ---------------------18
C.
Report amendments ------------------------------------------18
III) Justification of Test System
----------------------------------18
IV) Materials and Methods
-----------------------------------------19
A. Field
experiment -------------------------------------------19
1. Lineage and history
of seed used for field test------19
2. Plot
information
-----------------------------------19
3. Sampling for
analysis -------------------------------19
a. Leaf tissue
--------------------------------19
i. Initial leaf
sampling ------------19
ii. Monthly sampling
-----------------19
iii.Whole plant ----------------------20
b. Seed tissue
-------------------------------20
i. Bulk seed ------------------------20
ii. Analytical seed ------------------20
4. Field Monitoring
------------------------------------20
B. Processing
experiment --------------------------------------20
C. Analytical
experiment
-------------------------------------20
1. GUS ELISA
-------------------------------------------20
2. CP4 EPSPS ELISA
-------------------------------------21
3. GUS enzymatic
assay
--------------------------------21
4. CP4 EPSPS enzymatic
assay --------------------------21
5. Western blot assay
for CP4 EPSPS and GUS ------------22
6. Protein assay for
extracts (Bio-Rad assay) ----------22
7. Quality assays
--------------------------------------22
a. urease
----------------------------------------22
b. sugar analysis by
HPLC ------------------------22
c. nitrogen solubility
analysis ------------------22
d. tryptophan-alkaline
hydrolysis ----------------22
e. moisture
--------------------------------------22
f. cysteine and
methionine -----------------------22
g. amino acids -----------------------------------23
h. trypsin inhibition
----------------------------23
i. ash
-------------------------------------------23
j. fatty acid profiles
---------------------------23
k. fiber
-----------------------------------------23
l. fat -ether
extraction -------------------------24
m. total kjeldahl
nitrogen-protein ---------------24
n. phytic acid, by
ion-exchange -----------------24
o. carbohydrates
---------------------------------24
p. calories
--------------------------------------24
q. free and bound
isoflavones --------------------24
r. lectines
--------------------------------------24
8. Statistical
analysis onb Soybean seed quality data----25
9.
Protein/aminoacids in oil
assays--------------------25
10. Other circumstances
pertaining to the study and
protocol and SOP deviations ----------------------25
a. Field experiment-------------------------------25
b.
Processing experiment -------------------------25
c. Analytical experiment -------------------------26
V) Results and
Discussion -------------------------------------------26
A. Field
Experiment ----- -------------------------------------26
1.
Agronomic practices ----------------------------------26
2.
Field monitoring
------------------------------------26
3. Leaf
and plant sampling ------------------------------26
4.
Harvest ----------------------------------------------26
B. Processing
experiment --------------------------------------27
C. Analytical
experiment --------------------------------------27
1. Levels of
CP4 EPSPS and GUS proteins in Soybean
Leaves and seeds ----------------------------------27
2.
Quality analysis of raw Soybeans ---------------------28
a.
Proximate analysis --------------------- -------29
b.
Amino acid analysis ----------------------------29
c.
Fatty acid analysis ----------------------------30
d.
Isoflavone analysis ----------------------------30
e.
Lectin analysis --------------------------------30
f.
Trypsin inhibitor and urease -------------------31
3.
Proximate analysis of full-fat Soybean flour ---------32
4.
Quality analysis of toasted Soybean meal -------------32
a.
Initial preparation of toasted Soybean meal ----33
i.
Proximate analysis
----------------------33
ii.
Phytate --------------------------------33
iii.
Trypsin inhibitor,urease, and
nitrogen
solubility index --------------33
b.
Retoasted Soybean meal -------------------------34
i.
Proximate analysis
----------------------34
ii. Trypsin inhibitor, urease, and
nitrogen solubility
index ---------------34
iii. Laboratory cooking of Soybeans
Samples to test T1 inactivation
--------35
iv.
Phytate in retoasted meal ---------------36
v. Stachyose and
raffinose in retoasted
meal
-----------------------------------36
vi.
Lectins in retoasted meal --------------36
vii.
Isoflavones in retoasted meal ---------37
5. Expression of CP4 EPSPS and GUS in retoasted
Soybean meal---------------------------------37
a. SDS-extractions
and Western blot analysis --------37
b. Expression of CP4 EPSPS and GUS in protein
fractions from non-denaturing extracts
and Western blot, ELISA,and enzymatic
activity assays ----------------------------38
i. GUS
assays ------------------------------39
ii.
CPE EPSPS assays -----------------------39
6.
Analysis of Soybean oil------------------------------40
a. Fatty acid
composition of refined, bleached,
@@deodorized oil --- -----------------[[-------40
b. Determination of
protein/amino acid levels
@found
in refined, bleached, deodorized oil---40
VI) Conclusions
----------------------------------------------------42
VII) References
----------------------------------------------------43
VIII) List of
abbreviations-----------------------------------------50
LIST OF TABLES
Table 1. Chemical treatments used for glyphosate-torelant
Soybean field test
-----------------------------------------52
Table 2. Summary of Disease and insect monitoring
log.---------------52
Table 3. Plant tissuesampling log
-----------------------------------53
Table 4. Yield of Soybean seeds from 1992 Puerto Rico field
test-----53
Table 5. Puerto rico processing experiment shipping log
-------------54
Table 6. Expression of CP4 EPSPS and GUS in Soybean plant tissues,
determined by ELISA
--------------------------------------- -55
Table 7. Puerto Rico analytical experiment shipping log
-------------56
Table 8. Summary of Proximate analyses of Soybean seeds
-------------56
Table 9. Summary of amino acid analyses of Soybean seeds
------------57
Table 10. Summary of fatty acid analyses of Soybean seeds
-----------57
Table 11. Summary of isoflavones analyses of Soybean seeds
----------58
Table 12. Summary of lectin analyses of Soybean seeds
---------------58
Table 13. Summary of trypsin inhibitor and urease analyses
for
Soybean seeds ---------------------------------------58
Table 14. Analysis of full-fat soybean meal -------------------------59
Table 15. Analysis of toasted meal
----------------------------------60
Table 16. Analysis of retoasted meal
--------------------------------60
Table 17. Isoflavone analysis of retoasted meal
---------------------60
Table 18. Expression of CP4 EPSPS and GUS in retoasted Soybean
meal by multiple SDS
extractions using Western blots ----61
Table 19. Comparison of CP4 EPSPS and GUS expression in retoasted
meal and seeds
------------------------------------------62
Table 20. Expression of CP4 EPSPS and GUS in desalted retoasted
Soybean
meal extracts, and seed extracts,using a non-SDS
buffer
--------------------------------------------------63
Table 21. Fatty acid analysis of refined bleached deodorized oil
----63
Table 22. Summary of protein content of refined, bleached,
deodorized
oil ------------------------------------------64
Fig 1 Lineage of glyphosate-torelant Soybean
lines 61-67-1
and
40-3-2
----------------------------------------------64
Att.1 Protocol for
experiment 92-420-701 -----------------------66
Att.2 Protocol for experiment 92-419-712 -----------------------76
Att.3 Protocol for experiment 92-419-710 ------------------------93
Att.4 Protocol Amendments
---------------------112
Att.5 Processing report from Texas A &M University
-------------121
Att.6 GUS ELISA Validation data
Summary -----------------------143
Att.7 CP4 EPSPS ELISA Validation
Data Summary ------------------144
Att.8 Method development and
report of the determination of free
and bound isoflavones in soy products
--------------------145
Att.9 Method development and
report of the lection assay for
soybean seeds and meal
-----------------------------------154
Att.10 Statistical analysis of CP4 EPSPS and GUS expression in
Soybean seeds and leaves --------------------------------161
Att.11 Raw data sheets for quality analyses -------------------170
Att.12 Statistical analysis of quality data for soybean seeds---211
Att.13 Analysis of trypsin inhibitor levels of retoasted
soybean samples after laboratory
steaming ----------------216
Att.14 Determinations of Protein/Amino acids in Soybean Oil
by Amino acid Analysis -Data sheets
----------------------221
Att.15 Calculatiuons for Protein/Amiono acid in Soybean Oil
Recovery ------------------------------------------------229