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Morphine Extraction From Domestically Grown Opium Poppy

Morphine Extraction From Domestically Grown Opium Poppy

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sawdust offers a potential saving of 237cover manure, if material costs, overhead.and yields are the same. Where thesawdust would be available at no cost,the saving woulcl be
557,.
As
shown in the photographs,
P.
ostreatus
is very different from
A.
cum-pestris. Pleurotus
does not grow in thefamiliar button form characteristic
of
young
dguricus.
It does not have thethick “meaty” tissue of the
Agaricus
buttcns. In shape and growth
it
re-sembles more closely the Japaneseshiitake mushrocNm. Like the latter.it has a tough, inedible stem. Theflavor, hoivever,
is
more like that
of
A.
campestris. Plenrotus
Lvould appear tohave
its
greatest value as a flavoringingredient for soups, sauces, and graviesrather than as
a
fresh mushroom fortable
use.
hfushrooms are a source of essentialamino acids and of the B vitamins
(7.
4,
7,
8).
They can be “factory-pro-duced” the year around from wasteproducts which originate from non-
OPIUM
ALK,ALOIDS
depleting sources and may be visualizedas an important food source for thefuture. Full realization of the marketpotential, ho\vever, awaits more effi-cient production and lo\l-er cost.
Literature Cited
(1) Anderson:
E. E.:
Fellers.
C.
R..
Pror. Am. Soc. Hort.
Sci.
41,
301-4(1942).(2) Badcock,
E.
C.?
Brit. .tlwol.
Sor.
Trans.
25,
200-5 (1941).(3)
Ibid.,
6,
127-32 (1943).
(4)
Block?
S.
S.:
Stearns.
T.
\$:.-
Ste-phens?
R.
L.:
McCandless.
R.
F.
J..
J.
AGR. FOOD
CHEH.
1,
890-3 (1953).(5) Block,
S. S..
Tsao,
G..
129.h hleet-ing,
.4CS:
Dallas, Tex.. April 1950.(6) Dzvidson.
R.
A,.
Czrrpbell.
MT.
A,.
Elzisdell. D.
J..
J.
‘4gr.
Research
57,
(7)
Esselen.
\V.
B.. Jr.. Fellers.
C.
B..
.\lass.
.4pr.
Exb.
Sta.
Bull.
434.
1-11683-95 (1938).
Y
(1946).
Technol.
3.
355-6 (1949).(8) Humfeld. H.. Sugihara.
T.
G..
FGO~
(9)
Lambert,
E.
B..
Farmer‘s
Buil.
1875,
12 (1941).(10) Lambert,
E.
B., Ayers,
T. T.,
Plant
(1
1)
Niethammer,
A,,
Zentr.
Bakteri-
(12) Rempe,
H.,
Mushroom
Sci.
2,
Disease Reptr.
36,
261-8 (1952).
dog.
2,
129-30 (1942).131 (1953).(13) Sinden’,
J.
W.,
Pa.
Agr.
Expt.
Sta.Bull.
365.
1-27 (1938).(14)
Zbid.?
82,
1-26 (1946).(15) Sinden,
J.
W.:
Hauser,
E.,
Mush-room
Sri.
1,
52-9 (1950).(16) Stoller, B.
B.:
Plant
Phjsiol.
18,
397-414 (1943).(17) Thom,
C.,
Church,
hl.
B.,
“Thet\spergilli,”
p.
39. Williams
&
Wilkins,Baltimore, 1926.(18) Treschotv,
C.,
Danske Botan. .4rkiu.
11,
1-180 (1944).
(19)
Vaksman.
S.
A,,
Reneger,
C.
A.,
1tf)GoiogiQ
26,
38-45
(1
934).(20) M‘inters, R.
K.?
Chidester,
G.
H.,
Hall? J.
A,,
U.
S.
Dept,
rigr.
ForesfSeru.
Rept.
4,
\Vood Waste in
U.
S.
(1947).
Received
for
reuiew
May
7,
1958.
AcceptedSebtember
15.
1958.
Divtsion
of
Asricultural
old
Food
Chemistry,Dallar,
Tex.,
.4prd
1956.
729th
’Qeeting, ACS,
0.
1.
BREKKE,
G.
C.MUSTAKAS,J. E. HUBBARD, H.
G.
MAISTER,
1.
VAN
ERMEN,’
M.
C. RAETHER,and C.
T.
LANGFORD’Northern Utilization Research andDevelopment Division, U.
S.
De-partment
of
Agriculture, Peoria,
111.
To meet the needs of our nation in an emergency, a process was developed to recovercrude rnorphine liquor from mature, domestically grown, opium poppy plants.
This
liquorcan be used by licensed refiners as a substitute for opium to produce medicinal morphine,if
U.
S.
opium imports should be severely limited or cut
off.
Over
95%
of the morphinewas extracted from meal with water-saturated isobutyl alcohol in a continuous counter-current extractor.In preparing the meal, sterns and seed were separated from capsularmaterial by a four-step size-reduction procedure with a
6%
loss
of
morphine Morphineconcentration in the meal was increased from
0.5
to
o.7yO.
An aqueous ammonia treat-ment
of
the meal prior to extraction liberated the alkaloids from their naturally occurringsalts. Poppy meal or straw keeps in dry sforage without any morphine
loss.
MPORTED
OPIcni
is the source of me-
I
dicinal morphine in the UnitedStates.
To
ensure adequite suppliesof morphine in
a
national emergency.work \vas undertaken
tq
develop amethod
for
recovxing crule morphineliquor from the mature capsules
of
opiumpoppy plants gro\\n in the United States.Opium
is
the dried juice
or
latex ofunripe capsules of a particular poppyspecies,
Papaver .somn~eriirn.
.Althoughthe opium poppy has been grown forthousands
of
years: opium
is
still ob-tained through much tedious manualwork, both in cultivating the plant andin collecting the latex
(1).
ome 22
1
Present addresir,
281
1
Houston
Drive
*
Present address, 5646 Chelsea Are.,North,
La
hfarqur! Tex.
La
Jolla.
Calif.
alkalcids are found in opium. but onlythree-morphine. codeine. and papaver-ine-are of commercial importance. Theamount of morphine varies over widelimits, but in a good grade of opium tiecontent averages 10%. and t’le codeineand papaverine are present in muchsmaller amounts.Interest in cheaper producticnmethods led to the deirelopment ofmore modern processes
f
\r
recweringopium alkaloids directly Gm the rip-ened p3ppy plant. and some
of
theseprocesses
\cere
put into cqmmercialoperation on a very limited scale inGermany, Switzerland, and Hungar).in the 1930’s
(5:
6.
9).
From informa-tion given in the literature for these andother processes
(7).
each appears tohave disadvantages.
VOL.
6,
NO
Morphine Analyses.
All of thesamples were analyzed by the Matchettand Levine method
(77,
76),
but for arapid estimate, a modification of Hanes’ferricyanide micromethod for deter-mining reducing sugars
(-?)
was employed.Most analysts believe the Matchettand Levine method
is
insufficiently spe-cific for morphine
(76)
therefore, acommercial morphine refiner checkedduplicate samples from one of the ex-traction tests. The extract liquor wasexamined for
its
morphine content by amodified
U.
S.
Pharmacopoeia methodand a special method was used for thepoppy meal
(8).
Preparation
of
Poppy Meal.
Theopium poppy was grown under irriga-tion by the Field Crops ResearchBranch of the
U.
S.
Department of
12,
DECEMBER
1958
927
 
Agriculture. At maturity the crop washarvested with a conventional smallgrain combine modified to produce threefractions: poppy seed, stems, andleaves which were returned to theharvest field, and crude straw-a mix-ture of capsules, stems, and seed
(75).
The highest concentration of mor-phine is in the capsule of the plant, alittle is in the stems, but none is in theseed
(7).
Much less material needsprocessing if stems are separated fromthe capsules; because straw must beprotected from rain, such a separationreduces the investment for storage facili-ties. Seeds also should be removed,because their oil complicates morphinepurification.Preliminary milling studies indicatedthat a corrugated roller mill would pro-duce flattened, partially cut stems andbroken capsular material that could beseparated by screening. Because cap-sular material could not be rolled andflaked satisfactorily prior to solventextraction, as in oilseeds processing, itwas ground into a meal passing a 20-mesh sieve to facilitate extraction.Subsequently, the 4-break milling pro-cedure illustrated in Figure
1
was de-veloped and used to process a 4275-pound lot of crude straw. Details of themilling conditions are given in Table
I.
An
Allis-Chalmers experimental rollermill equipped with LePage corrugatedrolls measuring 6
X
6 inches was em-ployed for the first break and a 3-pair-highRobinson roller mill with
9
X
18 inchconventional corrugated rolls was usedfor the next three breaks. Normallyonly one pair of rolls with proper cor-rugations and speed differentials is usedfor each break. Because of equipmentlimitations, two pairs were used for thethird break and three pairs for the fourth.Any remaining oversize stock was groundin a
So.
000
Abbe mill operated at 700r.p.m. The Robinson rolls were op-erated sharp-to-sharp, but the cuttingedges were dull. The milled streamfrom each break was screened in aRobinson grain cleaner, size 2U, op-erated without aspiration and equippedwith screens having round-hole perfora-tions of the sizes shown in Figure
1.
The resultant poppy meal constituted697, of the crude straw, occupied
only
about one third the original volume, andhad a bulk density of about 13 poundsper cubic foot. The morphine lost inall discarded stems totaled only 5.77,of that present in the crude straw.Removing these stems decreased theweight of the meal to be extracted by
22%
and seed removal decreased itanother
6.5%.
In this way the mor-phine concentration in the meal was
in-
creased from approximately
0.5
to
0.7%.
If kept dry, the straw or meal canbe stored throughout the year withoutloss of morphine. Meal stored in both
Table
1.
Milling Conditions Used
for
Poppy Meal,
lot
MS-7
Clearance,
Fasf
Roll,
Slow
Roll,Break Type
of
Corrugafed
Roll
Inch R.P.M. R.P.M.
1
LePage corrugations, 5 per inch 0,025 380 342
2
Conventional, spiral cut corrugationsTop pair, 8 per inch 0.018 460 1803 Conventional, spiral cut corrugationsTop pair, 8 per inch
0.010
460 180Middle pair, 12 per inch 0,008 51 1
201
Middle pair, 12 per inch 0.005 511 2014 Conventional, spiral cut corrugationsTop pair, 8 per inch 0.008 460 180Lower pair, 20 per inch 0.002 575 225
Table
II.
Typical Conditions andValues
for
Extraction
of
Poppy Meal
Wetting liquor, rate. lb./hr. 20Meal (air-dry) feed rate, lb./hr. 12Solvent
A
rate, Ib./hr.
54
0
Solvent
B
rate,
lb./hr.
26
2
Over-all solvent ratio
67
Solids retention time withinextractor, min.
45
Extraction temperature.
F.
140Solvent feed temperatures,
O
F.
Fines removed
from
extractliquor, lb./100 lb. poppymeal
1
75
.\nhvdrous ammonia
rate.
lb.
/
135-140
,,
100
Ib. poppy meal 1.25
Figure
1.
Diagrammatic flowsheet
for
Morphine concentrationin
milling poppy straw
extract
liquor,
70
0
225
Figure
2.
Diagrammatic
CiA"*I"C,RIC
FCLDCII
pressing operations
n*r
flowsheet for extraction and
KCWNtn"
CXTEACIOR
open and sealed containers kept at roomtemperature and in an unheated barnshowed
no
loss of morphine in
2
years.
Extraction
of
Alkaloids.
Morphineconcentration in poppy meal is very lowcompared to the solute level in such ma-terials as oilseeds which ordinarily areextracted in large-scale continuous ex-tractors. However, it had been foundpreviously that a high percentage of themorphine could be extracted in
l'2
hour
(72,
73.
74)
;
this is well within apractical range for continuous extraction.Poppy meal wetted with extractliquor was fed through a gravimetricfeeder followed by a screw conveyorand into a continuous countercurrenthorizontal extractor of the Kennedytype
(70)
with 20 extraction stages.Poppy meal was introduced at stage
1.
and two solvent streams were used,one entering at stage 20 and the otherbetween stages 16 and 17. The extractedsolids were drained for approximately
7
minutes on an inclined flight conveyor.Extract liquor was filtered throughcloth bags made of cotton duck, style
8,
to remove suspended solid particles.The extraction equipment was opera-ted on a continuous basis for periodsof
20
to 24 hours.About
1
hour before the poppy mealwas fed into the extractor, 6-poundbatches were mixed with 10 pounds offresh extract liquor to which
150
ml.of aqueous ammonia
(23.370
"3)
hadbeen added. This treatment reducedthe quantity of fines carried in the ex-tract liquor and the ammonia liberatedalkaloids from their naturally occurringsalts.
A
diagrammatic flowsheet forthe extraction and pressing operations
is
shown in Figure
2.
Typical flow rates and process con-ditions established after a number ofexploratory runs are given in Tables I1and
111.
The resultant extract liquor contained96.9% of the morphine in the poppymeal feed. Increasing the amount ofwetting liquor decreased the yield
of
morphine somewhat and also increased
928
AGRICULTURAL
AND
FOOD
CHEMISTRY

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