WO2014153629A1

WO2014153629A1 - Automated solid phase extraction system

Info

Publication number: WO2014153629A1
Application number: PCT/BR2014/000058
Authority: WO
Inventors: Jarbas José Rodrigues ROHWEDDER; Ricardo Mathias ORLANDO
Original assignee: Universidade Estadual De Campinas - Unicamp
Priority date: 2013-03-27
Filing date: 2014-02-20
Publication date: 2014-10-02
Also published as: BR102013007167B1; BR102013007167A2

Abstract

The present invention relates to a solid phase extraction system comprising a level sensor that allows the presence and level of a liquid (solvents and samples) to be detected inside the cartridge, to determine the flow rate used to elute the liquid, and also to detect whether the liquid was completely eluted from the cartridge. This device comprises optoelectronic transmission keys that are coupled to the extraction cartridges in such a way that the logical signal from the device can be used by an electronic circuit in order to automate the various steps of solid phase extraction.

Description

AUTOMATED SOLID PHASE EXTRACTION SYSTEM

Field of the invention

The present invention relates to a device for coupling to solid phase extraction cartridges and solid phase extraction (SPE) systems which allows to detect the presence and level of liquid (solvents and samples) within the cartridge, to determine the flow rate employed for eluting the liquid and also detecting if the liquid has been completely eluted in the cartridge.

This device is based on transmissive optoelectronic switches composed of: an emitting photodiode and a collecting photodiode. By properly positioning the extraction cartridge between these two photodiodes, the intensity of light collected by the collecting photodiode will be dependent on whether or not liquid is present inside the cartridge. The variation in the intensity of light collected results in a variation in electrical voltage that can be used as a logical signal to drive a valve, vacuum pump or any other electro-electronic device employed in solid phase extraction systems. automated or semi-automated.

This semi-automated solid phase extraction system containing level sensors based on transmissive optoelectronic switches is primarily intended for chemical, pharmaceutical, food, biotechnology and agricultural laboratories and industries.

Fundamentals of the invention

Solid phase extraction (SPE) employing cartridges and discs represents a large portion of the sample preparation procedures due to the peculiar advantages of this technique (Spears, 2004).

Standard SPE procedures require four to five steps where different liquids (sample and solvents) pass through the cartridge or disc sorbent. During the first four steps of the extraction procedure it is of fundamental importance that the sorbent is always in contact with any liquid to prevent it from drying again. Other A very important caution is when it comes to the correct time to introduce solvents into the cartridge. When one solvent is being replaced by another the analyst should be careful not to over a very large volume of solvent above the upper cartridge filter.

These precautions aim to ensure repeatability and efficiency of sample preparation. When this procedure is performed manually with conventional manifold systems the need to maintain the liquid level by covering the extraction sorbent (solid phase) makes it very stressful to perform and makes it difficult or impossible to perform multiple extractions simultaneously. In this regard, mechanized, automated or semi-automated systems are preferably employed.

Automated or semi-automated systems employ solenoid valves, vacuum or peristaltic pumps, sensors (pressure, position, and movement) as well as liquid dispensing devices that can promote both liquid entry into and exit from the cartridges, employing little or no manual manipulation of the operator during the extraction steps.

Even for automated and semi-automated systems a major operational difficulty of the device is to properly control the liquid level within the extraction cartridge.

Some patents describe the use of cameras employing charge-coupled device (CCD) image sensors, laser devices, or devices with ultrasound or pressure sensors (Patents: JP2006007081 (A) - 2006-01 -12; EP1159597 (A1) - 2001-12-12; EP1 159597 (A1) - 2001-05-12; JP2005204578 (A) - 2005-08-04; JP2007298445 (A) - 2007-1-1-15).

Although capable of detecting the liquid level inside the cartridge, all of these devices have a number of disadvantages compared to the transmissive optoelectronic switches presented here. Among these disadvantages we can highlight: larger dimensions of these electronic devices, larger operating complexity, higher costs and difficulties to be coupled with any type of cartridge. For ultrasonic and pressure sensors, slight variations in the density and viscosity of the solvents employed may lead to erroneous measurements of the liquid level in the cartridge. Sensors represented by CCD or laser cameras cannot be used using metal or opaque cartridges and are relatively expensive devices.

All these difficulties and limitations are easily solved by using the transmissive optoelectronic switches known as optos. The simplicity of these electronic devices, their wide commercial range and their low cost make it possible for them to be employed as level detectors for solid phase extraction cartridges in a much simpler and cheaper way. The use of transmissive optoelectronic switches (if inserted inside the cartridge) also allows the use of cartridges connected in series or even cartridges with metal walls. Due to their small size and low cost optos can be coupled to dozens of cartridges at the same time whereas in fully automated commercial systems it is often possible to perform a maximum of 4 extractions simultaneously. Optos are also perfectly adjustable to various cartridge diameters, which is not generally possible with the other sensors employed in automated systems.

Brief Description of the Invention

This patent application relates to a semi-automated solid phase extraction system containing level sensors based on transmissive optoelectronic switches for coupling to cartridges and solid phase extraction discs and solid phase extraction systems.

This system consists basically of:

(a) conventional or adapted transmissive optoelectronic switch containing a light emitting diode and a light collecting diode 1.1 and 1.2. b) bracket or guide provided for the transmitter and collector photodiodes in addition to the proper coupling and positioning of the solid phase extraction cartridge 2.1 and 2.2.

c) a conventional solid phase extraction cartridge or adapted with markings or modifications to the cartridge wall surface to facilitate positioning of opto 3.1 and 3.2.

d) an electronic circuit for input and monitoring of the signal from the sensor.

The present invention further comprises the use of the level sensor described for any solid phase extraction process whether or not coupled to negative pressure systems (vacuum pump and peristaltic pump) or positive pressure system.

Brief Description of the Figures

Below is a brief description of the accompanying figures for the purpose of facilitating the understanding and understanding of this application, which should not be construed to limit the scope of protection of the present technology.

Figure 1 shows a schematic representation of a conventional transmissive optoelectronic switch with the light emitter and light collector regions 1.1 and 1.2.

Figure 2 shows a schematic representation of the snap-on bracket or guide for coupling the solid phase extraction cartridge.

Figure 3 shows a schematic representation of a conventional solid phase extraction cartridge and an example of cartridge modification (protrusion) to facilitate sensor positioning.

Figure 4 shows a schematic representation of an electronic circuit composed by the transmitter and collector photodiode as well as an operational amplifier and the logic signal output.

Figure 5 shows a schematic representation of a 5.1 solid phase extraction cartridge positioned in the photoactive region of optoelectronic switch 5.2 by the aid of holder 5.3. Figure 6 shows a schematic representation of an SPE cartridge coupled with three different optoelectronic switches simultaneously 6.1.

Figure 7 shows a schematic representation of an optoelectronic switch that has been modified by coating the photodiodes with solvent resistant polymeric material and which can be introduced into the solid phase extraction cartridge.

Figure 8 shows a prototype representation of the automated extraction system with details for the optoelectronic switch fitting trails 8.1, the brackets for positioning the extraction cartridges with the optoelectronic switches 8.2, and the region where the cartridges will connect to the extraction 8.3.

Detailed Description of the Invention

This patent application refers to a semi-automated system containing level sensors based on optoelectronic switches that allows to detect the presence and level of liquids (solvents and samples) inside the cartridge, to determine the flow rate employed for the elution of the liquid and also detect if the liquid has been completely eluted in the cartridge. Employing this device coupled with electro-electronic circuits, the voltage variation signals of the photo diode collector can be used to control the activation of pressure systems, open and close valves, multi-valves and others in order to automate the operation. procedure and reduce both the operational errors and the stress of the analyst while performing the extraction.

The invention uses as a basic inventive element the implementation of a transmissive optoelectronic or opto switch, which has as main components in its construction an emitting photodiode and another light collecting photodiode, which are kept at a suitable distance from each other. These two components are supplied with an appropriate voltage to cause the emitting photodiode to radiate light relatively steadily over the collecting photodiode. The light Focusing on the photodiode collector causes its electrical resistance to be changed causing a variation of electrical voltage (low level).

When the liquid material is positioned between the two photodiodes by absorptive, reflective and scattering processes, part of the electromagnetic waves that should focus on the collecting photodiode do not reach this component. This reduction in the amount of light reaching the collector photodiode causes the electrical resistance of this diode to change and thus increase and difference in electrical voltage between its terminals. This variation in electrical voltage can be used as a control signal for various unit operations during the extraction process.

In the case of solid phase extraction steps what will cause the variation of the control signal intensity will be the presence of liquid or air inside the cartridge in the portion monitored by the optical switch. In order to be able to observe such variation of the optical switch signal the cartridge must be properly positioned between the two photodiodes so that the processes of light absorption, reflection and scattering take place properly. Correct positioning of the cartridge with the opto causes the change from liquid to air and vice versa generates a transient logic signal that can be employed for the purposes described above.

Since conventional optical switches are not designed for coupling solid phase extraction cartridges, a holder must properly position them. Such supports shall be capable of adapting to different cartridge diameters and shall have elements enabling the cartridge to be properly positioned and leveled as colored marks and / or holes and / or grooves and / or protuberances, etc. Cartridges may also have similar elements that facilitate positioning and leveling. The support can also be made of a single piece that joins in its structure the two diodes of the optical switch.

Commercial optical switches are generally small devices, which allow simultaneous coupling of multiple optical switches in the same cartridge or in series-coupled cartridges. The number of optical keys employed during the extraction process, as well as their placement in the cartridge, may vary as needed. An optical switch positioned in the reservoir just above the cartridge upper filter prevents the sorbent from drying out (Figure 6.1). Two optical switches positioned above the sorbent allow you to accurately measure the flow rate employed (Figure 6.1 and 6.2). An optical switch positioned on the cartridge outlet (nozzle) lets you know if the cartridge has dried properly during the drying step (Figure 6.3).

For the correct operation of the optos, in principle, they must be coupled externally to the extraction cartridge. It is also necessary that the cartridge wall be made of transparent or translucent material.

In cases where metal body cartridges are used, conventional transmissive optoelectronic switches may be modified. For cases of opaque walled cartridges this application proposes the use of adapted keys that can be inserted into the extraction cartridges. These keys differ from conventional keys in that emitting and receiving photodiodes are enclosed in a capsule of transparent or translucent solvent resistant material. Such capsules may be composed of plastics or glasses resistant to solvent attack and sufficiently capable of allowing adequate light to pass through.

The features previously described for the transmissive optoelectronic switch-based level sensor for solid phase extraction cartridges represent a constructive simplification of the level sensors already described.

The invention, which is the subject of this document, is within the context of sample preparation techniques, more specifically solid phase extraction techniques employing cartridges or discs. This document deals with a semi-automated level control system used for manifold or robotic systems (workstation) for solid phase extraction, which basically consists of: The. Metal or plastic valves and / or piping connected at one end to a solvent propellant system such as a peristaltic pump, syringe pump or vacuum pump and the other end connected to the cartridge outlet (nozzle).

B. at least one conventional transmissive optoelectronic switch to be coupled to the solid phase extraction cartridge reservoir just above the upper filter (Figure 1);

ç. at least one holder or guide for engaging, aligning and correctly positioning the solid phase extraction cartridge with the transmissive optoelectronic switch (Figure 2);

d. at least one track or guide for engagement, alignment and correct positioning of the transmissive optoelectronic switch with the extraction system (Figure 8);

and. at least one bracket or guide for engagement, alignment and correct positioning of the transmissive optoelectronic switch with the extraction cartridge (Figure 2);

f. at least one conventional solid phase extraction cartridge (Figure 3);

g. at least one electronic circuit capable of amplifying, receiving, sending or distributing the signal from the optoelectronic switch (Figure 4);

The present patent application further comprises the use of the described devices for any solid phase extraction process.

In this system it also comprises the following constructive variables: a) The system may have propellant systems or solvent flow controllers which may be peristaltic pump, vacuum pump, syringe pump, solenoid valves or step motors coupled to the cartridge outlet or inlet. extraction by means of pipes of any nature and whose operation is controlled or modulated by the signal from the optoelectronic switches; (b) Transmitting optoelectronic switch emitting and collecting photodiodes may be coated with solvent resistant material such as glass or polymers so that they can be inserted into the cartridge (reservoir) (Figure 7);

c) Extraction cartridges may receive any variation in their shape, color, texture or relief shape from their inner and outer walls to facilitate positioning and alignment of the cartridge with the optoelectronic switch (Figure 3); d) The extraction cartridges can be coupled simultaneously to two or more optoelectronic switches so that it is possible to determine the flow during extraction (Figure 6);

e) The optoelectronic switches can be coupled to the extraction cartridges through the nozzle or extraction cartridge outlet to control the drying step (Figure 6); f) The solid phase extraction system employing the devices described herein may have one or more steps in the automated extraction process controlled or modulated by the signal from the transmissive optoelectronic switch.

Embodiment Example

The transmissive optoelectronic key-containing solid phase extraction system to which this patent refers has been constructed as follows:

Each transmissive optoelectronic switch described in Figure 1 was connected to an amplifying electronic circuit as described in Figure 4 and to an electrical power supply.

The transmissive optoelectronic switches were coupled to the extraction system by two tracks positioned on a plate allocated behind each row of extraction cartridge (Figure 8.1).

Each optoelectronic switch has been fitted with a bracket for its correct alignment and positioning with the extraction cartridge (Figure 8.2). Correct positioning of the cartridge with the optoelectronic switch was performed fitting the cartridge reservoir portion between the two photodiodes of the optoelectronic switch.

The extraction cartridges were simultaneously coupled to the extraction system and the optoelectronic switch holder. Attachment to the extraction system was accomplished through connections of the extraction system to the cartridge nozzle (Figure 8.3). The holder was already fitted to the cartridge body more precisely in the reservoir portion just above the upper filter.

Signals from the transmissive optoelectronic switch in response to air and liquid variations within the cartridge were transmitted to a parallel interface of a microcomputer by means of metal cables.

A computer program used the signals from the optoelectronic switches to turn solenoid valves and a peristaltic pump on and off to control flow and elution during the various stages of solid phase extraction.

Alternatively the conventional commercial optoelectronic key was developed a modified optoelectronic key by introducing the conventional key diode photos into polytetrafluoroethylene plastic tubing (Figure 7). This modified optoelectronic key was inserted into the solid phase extraction cartridge and with it obtained results similar to those of the commercial optoelectronic key externally coupled to the cartridge wall.

Claims

Automated system for solid phase extraction characterized by comprising at least one level sensor for solid phase extraction cartridges based on transmissive optoelectronic switches.

Automated system for solid phase extraction characterized by comprising:

a) conventional or adapted transmissive optoelectronic switch containing a light-emitting diode and a light-collecting diode 1.1 and 1.2;

b) support or guide provided with a fitting for the emitting and collecting photodiodes in addition to the appropriate coupling and positioning of the solid phase extraction cartridge 2.1 and 2.2;

c) a conventional or adapted solid phase extraction cartridge with markings or modifications on the surface of the cartridge wall to facilitate positioning of opto 3.1 and 3.

two;

Automated system for solid phase extraction characterized by comprising:

a) Metal or plastic valves and/or pipes connected by one end to a solvent propellant system such as a peristaltic or vacuum pump and the other end connected to the cartridge outlet (nozzle).

b) at least one conventional transmissive optoelectronic switch to be coupled to the solid phase extraction cartridge reservoir just above the upper filter (Figure 1);

c) at least one support or guide for fitting, alignment and correct positioning of the solid phase extraction cartridge with the transmissive optoelectronic switch (Figure 2); d) at least one track or guide for fitting, alignment and correct positioning of the transmissive optoelectronic switch with the extraction system (Figure 8);

e) at least one support or guide for fitting, alignment and correct positioning of the transmissive optoelectronic switch with the extraction cartridge (Figure 2);

f) at least one conventional solid phase extraction cartridge

(Figure 3);

g) at least one electronic circuit capable of amplifying, receiving, sending or distributing the signal from the optoelectronic switch (Figure 4);

4. Automated system for solid phase extraction, according to claim 3, characterized in that it can have propellant systems or solvent flow controllers that can be a peristaltic pump, vacuum pump, syringe pump, solenoid valves or coupled stepper motors to the exit or entry of the extraction cartridges through pipes of any nature and which have their operation controlled or modulated by the signal coming from the optoelectronic switches.

5. Automated system for solid phase extraction, according to claim 3, characterized in that the emitting and collecting photodiodes of the transmissive optoelectronic switches can be coated with solvent-resistant material such as glass or polymers so that they can be inserted inside the cartridge (reservoir) (Figure 7).

6. Automated system for solid phase extraction, according to claim 3, characterized in that the extraction cartridges can receive any variation in their shape, color, texture or shape of the relief of their internal and external walls in order to facilitate positioning and aligning the cartridge with the optoelectronic switch (Figure 3).

7. Automated system for solid phase extraction, according to claim 3, characterized in that the extraction cartridges can be coupled simultaneously to two or more optoelectronic switches so that it is possible to determine the flow rate during extraction (Figure 6).

8. Automated system for solid phase extraction, according to claim 3, characterized in that the extraction cartridges can be coupled externally to the solid phase extraction cartridge by positioning the nozzle or output of the cartridge between the emitting and receiving photodiodes for the purpose to control the drying stage (Figure 6).

9. Automated system for solid phase extraction, according to claim 3, characterized in that the solid phase extraction system employing the devices described herein can have one or more steps of the automated extraction process, controlled or modulated by the signal from the transmissive optoelectronic switch.