US3620681A

US3620681A - Apparatus for extraction of drugs and toxic substances from blood, serum and other liquid

Info

Publication number: US3620681A
Application number: US863892A
Authority: US
Inventors: Eric S Wright
Original assignee: ERIC S WRIGHT
Current assignee: ERIC S WRIGHT
Priority date: 1969-10-06
Filing date: 1969-10-06
Publication date: 1971-11-16
Anticipated expiration: 1988-11-16

Abstract

Said apparatus is housed on and in a convenient metal frame. It has three extraction chambers arranged vertically. It extracts the desired drug or toxic substance from the sample with a suitable solvent. This extraction is carried out in the upper extraction chamber, after which the solvent is filtered into the midextraction chamber, and the sample or aqueous phase is retained. The middle extraction chamber contains carbon black, some other adsorbing agent or aqueous solution which effects the purification of the solvent. The solvent is filtered a second time into the lower extraction chamber where the desired drug or toxic substance is reextracted from the solvent into an acidic or basic solution, depending on its chemical nature. The actual extractions and purification are effected by a shaking motion of the extraction chambers, and all operations (extractions, purification and filtrations) are done automatically according to a predetermined program.

Description

D United States Patent [1113,620,681

[72] Inventor Fzle S. Wright 3,226,407 12/ 1965 Bergman .l 23/267 X 14947 Clymar St., Compton, Calif. 90220 3,259,462 7/1966 Anscherlik 23/259 X [2]] Appl. No. 863,892 3,348,921 10/1967 Katz 23/259 [22] Filed Oct. 6, 1969 3,403,980 10/1968 Litterio 23/259 X [45] Patented Nov. 16, 1971 3,415,380 12/1968 Ellis 23/259 X FOREIGN PATENTS s41 APPARATUS FOR EXTRACTION or DRUGSAND 328 :33; gg z gggg Toxic SUBSTANCES FROM BLOODSERUMAND 443 232 1912 France y m 23/272 om uQUm 2 Claims, 4 Drawing Flu. Primary ExaminerNorman Yudkoff 521 US. cl. 23/267 c, EmeY 210/322 ABSTRACT: Said a paratus is housed on and in a convenient P [51] Int. CL Bold 11/02, metal frame It has three extraction chambers arranged veni Bold 11/04 cally. lt extracts the desired drug or toxic substance from the [50] Field of Search 23/267, sample with a suitable solvent This extraction is carried out in 259, 292, 272, 312 S, 312 A, 3 l2 R, 312 ME, the upper extraction chamber, after which the solvent is fil- 3] 1; 210/ 322 tered into the midextraction chamber, and the sample or aqueous phase is retained. The middle extraction chamber contains carbon black, some other adsorbing agent or aqueous [56] CM solution which efi'ects the purification of the solvent. The sol- UNITED STATES PATENTS vent is filtered a second time into the

lower extraction R

2 ,13 611E5- aygn9g l. 231259 chamber where the desired drug or toxic substance is reex- 833,573 10/1906 BecigneuL. 23/312 S tracted from the solvent into an acidic or basic solution, de- 9|2.634 2/ 1909 Warburton 210/252 X pending on its chemical nature. The actual extractions and pul,890,939 12/1932 Fahmey 23/259 rification are efi'ected by a shaking motion of the extraction 2,136,372 1 H1938 Burnett 23/272.5 X chambers, and all operations (extractions, purification and fil- 2,968,721 1/1961 Shapiro 23/272 X trations) are done automatically according to a predetermined 3,206,276 9/1965 Bur-well 23/312 ME program.

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BY 6B4 I APPARATUS FOR EXTRACTION F DRUGS AND TOXIC SUBSTANCES FROM BLOOD, SERUM AND OTHER LIQUID BRIEF SUMMARY OF THE INVENTION The invention was designed to carry out many of the manual operations involved in the extraction of drug or toxic substances from blood, serum or other aqueous solutions. In addition to making a more thorough extraction, it has the capacity to complete many extractions simultaneously and thereby save time. More specifically, it makes the extraction of the desired substance from the sample into a solvent of choice that is more dense than the sample. After extraction, a brief period is allowed for complete separation of the solvent and sample. Then the solvent is filtered and purified in a separate chamber with an adsorbing-agent or suitable solution. Next, it is separated from the purifying agent and filtered again. Finally the desired substance is extracted from the solvent with acidic or basic solution, depending on its chemical nature, and reserved for spectrophotometric or other analysis. All operations mentioned are done automatically in turn by a predetermined program.

BRIEF DESCRIPTION OF THE SEVERAL VIEWS FIG. 1 is a view of the programmer unit from the rear. It shows the physical arrangement of the cam and the microswitches activated by it. The programmer motor, which drives the cam is not shown although it is attached underneath the programmer shelf. Also the electrical wiring is not shown in the view.

FIG. 2 shows the side view of the extraction panel when viewed from the right side. In this view, the suspension of said panel is shown. Also the arrangement of the solenoids, for opening the upper and middle extraction chambers is shown. And the solenoid for opening the upper extraction chamber is not shown since it may clutter the view of the upper rocker arms.

FIG. 3 shows the front of the apparatus. It presents a view of the control panel on the left, on which is mounted the programmer indicator lamp-part 11, the master switchpart 15, the fusepart l6, and the activator button-part 13. On the right side of the apparatus the extraction panel is obvious. It shows the three extraction chambers with funnels fitted at the top of the lower and middle chambers. Also the suspension of the extraction panel is shown by the attachment of the rocker arms to the panel and to the frame. The rocker arms in this view are behind the extraction panel but in front of the frame. A section of the frame is cut away on the right side of the apparatus to enhance the view of the shaker motor-part 10. The base of the shaker motor is also seen in this view. The pushrodpart 25, which is connected to the crank of the shaker motor and to the rear of the extraction panel is also shown.

FIG. 4 merely shows the schematic diagram of the electrical circuit.

DETAILED DESCRIPTION The detailed description of the invention is divided into two parts:

PART 1 explains construction of the invention.

PART II explains operation of the invention.

PART I-CONSTRUCTION FRAME The above-mentioned apparatus is mounted on a frame 25 inches tall, 12 inches wide and 8 inches deep. The material of construction of said frame is l l inches angle iron. Two more pieces of said angle iron are attached to frame, crosswise, in front and back and 6 inches up from the bottom. The purposes of these are to hold a shelf on which the programmer unit is mounted, and the front piece also serves as the base to which a moving part is attached. Said moving part will be explained later. A piece of channel iron, 1%X% inches is attached to the frame on the left side, running depthwise, and the top side of the channel is 9% inches below the top of the frame. The purpose of this is to serve as a motor mount for a geared electric motor whose one quarter inch shaft ends in a crank with a three-eighth inch displacement. See part No. 10, FIG. 3. The frame may be fastened together by bolts, rivets or welding, preferably welding. Also, a piece of 2$ 4%Xl/l6 inches stainless steel or aluminum is attached to the front right side of the frame in a lengthwise manner. This runs the entire length of the frame, and is referred toss the control panel. See part 26, FIG. 3. On this control panel is mounted the fuse holder (part 16, FIG. 3), the programmer motor indicator lamp (part 11, FIG. 3), the master switch (part 15, FIG. 3) and the activatorbutton (part 13, FIG. 3).

PROGRAMMER UNIT The programmer unit controls all the operations of the apparatus. It consists of a double pole relay (part 14, FIG. 4), a timer motor with a speed of l revolution per 30 minutes, a 3%- inch diameter cam driven by the timer motor. The timer cam has a raised portion which extends three-sixteenths inch out beyond the diameter and subtends an arc of 42. This raised portion activates the microswitches arranged around it, for a duration of 3% minutes each, when the timer motor is in operation. There are six microswitches (parts I-6, FIG. 1) arranged radially around, and each activated in turn by the programmer cam (part 7, FIG. 1). All operations of the program are carried out in one 30 minute revolution of the cam. The timer motor is mounted underneath the programmer shelf and is not shown except in the schematic diagram (see part 12, FIG. 4). However, the shaft of said timer motor extends upward through the shelf and turns the programmer cam in a clockwise direction. The overall function of the programmer unit will be covered in the description of operation.

EXTRACTION PANEL The extraction panel is a piece of stainless steel or aluminum 24X4% inches. (See part 24, FIGS. 2 and 3). Its purposes are twofold:

A. it serves as a base to which'the three extraction chambers are attached, with clamps as shown,

parts

18, 19, and 20, FIGS. 2 and 3. The upper and midextraction chambers are sealed at the bottom by a rubber policeman mounted at the end of a spring loaded lever. Both levers are referred to by the same part number (21 FIGS. 2 and 3. Also at the proper time in the program, each lever is activated by the solenoid (part 9, FIG. 2). The solenoid for the upper extraction chamber is not shown. When the upper extraction chamber (part 18, FIGS. 2 and 3) or the middle extraction chamber (part 19, FIGS. 2 and 3) is opened by the solenoid activated lever, the fluids in the chamber are permitted to drain out and into the 8 cm. funnel which is fitted with 10 cm. filter paper. The upper extraction chamber is sealed at the top by a Teflon stopper as shown. And the middle and lower extraction chambers are fitted at the top with Teflon stoppers, each of which is bored through and fitted with an 8 cm. funnel as shown. Each funnel shares the same part number (23), FIGS. 2 and 3. The lower extraction chamber (part 20, FIGS. 2 and 3) is sealed at the bottom by an appropriately attached stopcock as shown.

B. The second purpose of the extraction panel is to oscillate from right to left or vis a vis. This oscillatory motion (240 oscillations per minute) shakes the extraction chamber which effects the extraction or washing action as the case may be according to the program. The extraction panel is suspended from the frame by three rocker arms, each being referred to by the same part number (22), FIGS. 2 and 3. The rocker arms are steel, 4X$Xs inches, with holes drilled at each end with a distance of 2% inches between centers.

Also the rocker arms are fitted with 54-inch rivets or other suitable bearings. The upper end of each arm is fitted to the frame and the lower end is fitted to the extraction panel. FIGS. 2 and 3 show the connections of the rocker arms to the frame and extraction panel. Two of the arms are used near the top, and the third one is used near the bottom. The oscillation or shaking motion is provided by an electric motor with a gear reduction mounted at the lefi of the frame. See part 10, FIG. 3. This 240 r.p.m. motor has a one-quarter inch shaft that ends in a crank with a three-eighth inch displacement. The crank is connected to the extraction panel, near its center of gravity, with a ZXBXifi inches pushrod (part 25, FIG. 3).

ELECTRICAL CIRCUTI The electrical circuit is shown schematically in FIG. 4. The power comes through a standard 110 volt plug with a ground (part 17, FIG. 4). Next, it passes through the double pole single throw master switch (part 15, FIGS. 3 and 4). Also a ampere fuse is incorporated into the circuit (part 16, FIGS. 3 and 4). All operations are completed in a 30 minute cycle which stops as soon as the raised portion of the programmer cam opens the cut ofi microswitch (part 6, FIGS. 1 and 4). This particular microswitch is a single pole double throw type. And one of its purposes is to cut off the programmer cam motor (part 12, FIG. 4). After the cam engages, it is in the position shown in FIG. 4. To begin the next cycle, the activator button is pushed. The activator is a push button, two point make switch, and an instantaneous touch is all that is needed to engage the double pole, double throw relay (part 14, FIG. 4). As shown in FIG. 4, the relay is in the open position, but it is closed as soon as the activator is pushed and remains closed although the activator is released. In the closed position, current passes through the cutoff microswitch and through the bottom pole of the relay to keep the relay coil energized. Also, in the closed position, current passes through the cutoff microswitch through the top pole of the relay and energizes the programmer motor (part 12, FIG. 4) and the programmer indicator lamp (part I 1, FIGS. 3 and 4). As soon as the raised portion of the programmer cam passes and disengages the eutoff microswitch, it goes to its normally closed position which disengages the relay and energizes the programmer motor and indicator lamp directly. Stated briefly, the purpose of the relay and two point make pushbutton is to keep the programmer in operation until after the cam has passed the cutoff microswitch. At this point, the raised portion of cam is approaching the first microswitch to begin all operations of the new cycle.

Parts l,2,3,4 and 5, FIGS. I and 4 are all normally open microswitches. They are each activated by the cam in their 'tum to accomplish the automatic operations of the program,

which are:

Microswitch (I) energizes shaker motor for 3% minutes. The microswitches are spaced to allow an 8 minute delay between microswitches I and 2. Microswitch (2) activates the solenoid that opens the bottom of the upper extraction chamber (part 18, FIGS. 2 and 3). Microswitch (3) energizes the shaker motor for another 3 /5 minutes. Microswitch (4) activates the solenoid that opens the bottom of the middle extraction chamber (part 19, FIGS. 2 and 3). Microswitch (5) energizes the shaker motor for the third and final 3% minute period. Microswitch (6) cuts off the programmer motor and ends the cycle.

MANUFACTURING The apparatus shown in this specification is a single unit which handles a single sample at a time. It is desired that this apparatus be manufactured with multiple units combined on a single frame. This arrangement could be effected using the same electrical circuit and components except a motor of larger horsepower would be required for the shaker. If manufactured in multiple unit arrangement, this apparatus would be capable of making many simultaneous extractions in the same time required to complete a single extraction.

PART II-OPERATION A. For acidic or basic substances.

The operation begins by placing an appropriate volume of sample (2-7 ml.) into the upper extraction chamber (part 18, FIGS. 2 and 3). Also add to the same chamber a volume of solvent equal in size to 10 times the sample. The solvent must have a density greater than that of the sample. Both funnels (parts 23, FIGS. 2 and 3) are fitted with I0 cm. filter paper. A match head size portion of activated carbon is added to the middle extraction chamber (part 19, FIGS. 2 and 3), and a final solution is added to the lower extraction chamber (part 20, FIGS. 2 and 3). A convenient volume of final solution is 5 ml. If the drug or substance to be extracted from the sample is acidic in nature, then the final solution should be basic. If said drug or substance is basic in nature, then the final solution should be acidic.

The apparatus is now ready to operate and the activator button is pushed. The first operation is the extraction panel will be shaken, which will extract the desired substance from the sample into the solvent.

After the first extraction, an 8 minute waiting period is allowed by the program to permit good separation of the aqueous and solvent phases. Next, the bottom of the upper extraction chamber is opened automatically and the solutions drain out. The solvent, being heavier, drains first. It goes through the filter paper and into the middle extraction chamber, (part 19, FIGS. 2 and 3). Ifthe sample is blood, it will either remain in the upper extraction chamber or be caught on the filter paper. If the sample is any other aqueous solution, it will be absorbed by the filter paper. With this in mind, ample filter paper should be used in the funnel fitted to the middle extraction chamber.

After draining and filtration, the extraction panel will again be shaken. This is to permit the carbon black to adsorb certain impurities which may be present. This particular shaking operation, as well as the other two, lasts for a duration of 3% minutes.

After shaking the bottom of the middle extraction chamber, it is automatically opened, permitting the solvent to drain out and through filter paper and funnel into the bottom extraction chamber, part 20, FIGS. 2 and 3.

Next, the extraction panel is automatically shaken a third and final time. This shaking effects the extraction from the solvent and into the final solution. After the last extraction, the apparatus cuts itself off. After this, the solvent may be manually drained from the lower extraction chamber (part 20, FIGS. 2 and 3) and discarded. Next, the final solution, containing the extracted substance, is drained out of the lower extraction chamber for spectrophotometric analysis or other disposition.

B. For Neutral Substances.

The procedure and operations for the extraction of neutral substances are the same as for acidic and basic substances, except there is no final solution into which the extracted substance goes. It stays in the solvent phase. Also in the case of neutrals, the middle and lower extraction chambers are used to effect purification or washing of the solvent extract. One chamber may be used to hold acid solution and the other may be used to hold basic solution, or the middle and lower extraction chambers may be used to hold any other wash solutions or compounds, depending on the nature of the neutral compound and the sample from which it is extracted.

C. Metal Cones.

Two metal cones are prepared to fit into the funnels after they have been fitted with the filter paper. Also the vertex of each cone is cut off to permit fluid passage through the cone. A cone is fitted into either funnel when an aqueous solution, either wash or sample, is used in the extraction chamber above it. The purpose of the cone is to prevent the aqueous solution from touching the filter paper until all the solvent has gone through.

It is claimed that this invention will do two things. They are:

l. Extraction apparatus comprising three vertically serially arranged extraction vessels, said vessels each having a top opening and a bottom opening, first and second normally closed valves in the bottom opening of the top vessel and middle vessel respectively, a valve in the bottom opening of the bottom vessel, first and second filters disposed between the top and middle vessels and the middle and bottom chambers respectively, each filter being adapted to receive material discharged through the bottom opening of the vessel directly above it and to discharge filtered material through the top opening of the vessel directly below it, a vertical panel, said vessels, filters, and valves being mounted on said panel, motor means connected to said panel to provide oscillating shaking motion of said panel, and timer-control means operatively connected with the motor means and valve means to provide in sequence the steps of actuating the motor means to shake the panel and mix material in the top vessel, deactuating the motor means to provide a settling period, opening the first valve to allow material to drain out of the top vessel into the first filter and filtrate thence into the middle vessel, actuating the motor means, and opening the second valve to allow material to drain out of the middle vessel into the second filter and filtrate thence into the bottom vessel.

2. The apparatus of claim 1, wherein the timer-control means is arranged to provide the additional step of actuating the motor means to shake the panel and provide mixing of the filtrate passed into the bottom vessel.

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