JPS5972058A - Quick detection of medicine in urine - Google Patents

Abstract

PURPOSE:To detect quickly the medicine in urine with high accuracy by filtering the urine to be inspected with a polysulfone semipermeable membrane then adding an alkali metal halide particularly to the urine to be inspected or filtering the urine with the polysulfone semipermeable membrane after adding the alkali metal halide then extracting the same with a solvent. CONSTITUTION:A polysulfone semipermeable membrane is used for the filter membrane of a filter with a pressurization device, and the urine to be inspected is filtered without stirring under the pressure of gaseous N2. If salt such as NaCl, CaCl2 or the like is added at about 0.5-30% to the urine to be inspected, the material, acting as the surfactant in the urine grows to the size at which it cannot permeate the membrane. The urine is thus filtered in a short time without clogging the membrane. Ether is added to the filtered urine and after the urine is vigorously shaked, the urine is allowed to rest and the presence or absence of any medicine, for example, a narcotic, stimulant, cardiac, etc. extracted in the ether layer is detected. Since the surfactant is removed, the separability between the solvent layer and the water layer is fast with a good liqid separating condition and the time for the treatment is considerably shortened.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an improved method for detecting drugs in urine. In particular, the present invention relates to a method for quickly determining whether an individual is using drugs such as narcotics, stimulants, stimulants, cardiotonic drugs, and sedatives.

Conventionally, to detect drugs in urine, a solvent was added to collected urine, shaken, and then allowed to stand for separation, and drugs were extracted into the solvent layer and analyzed. The drugs to be tested are strong physiologically active substances, and many substances generally exhibit high polarity. In the extraction operation, quantitative recovery of the drug into the solvent layer cannot be expected, and it is necessary to use a large amount of solvent and repeat the extraction operation several times.

In this case, it takes time and effort to concentrate the solvent layer and bring the drug concentration to a detectable concentration.

In addition, urine generally contains surfactant components, and due to the influence of the surfactant components during separation by shaking with a solvent, the interface between the water layer and the solvent layer becomes unclear, and the urine is left standing for several hours for separation. Sometimes you have no choice but to do it.

If this separation is performed incompletely, the accuracy of quantitative analysis will be significantly reduced.

That is, conventional analytical methods have drawbacks such as problems in the working environment due to the use of large amounts of solvents, limitations on the number of specimens to be processed due to long pretreatment times, and problems in terms of analysis accuracy.

In these conventional analytical methods, it is known that the state of liquid separation can be improved by removing surface active components in dust. Therefore, a pretreatment method has been reported in which a cellulose acetate semipermeable membrane is used for filtration treatment to remove surfactant components onto the membrane surface, and the permeate is subjected to solvent extraction.

This method is an improvement over the conventional method in that most of the surfactant is removed and the standing time during solvent extraction is greatly shortened and the amount of solvent is reduced. However, because this method uses a cellulose acetate semipermeable membrane with a small pore size and a molecular weight cutoff of approximately 4,000, its water permeability is low, and the membrane can become clogged due to subtle compositional fluctuations in solute components in urine. However, there is a drawback that the membrane processing time is greatly extended depending on individual differences in urine, storage conditions after collection, and storage period.

The present invention aims to overcome the above-mentioned drawbacks, drastically shorten the pretreatment time for drug analysis in urine, and perform safe and rapid drug analysis by reducing the amount of extraction solvent. It is something.

In view of the results of the cellulose acetate semipermeable membrane described above, the inventors selected and tested a semipermeable membrane with a high water permeation rate as a separation membrane used for removing surfactant substances in urine.

As a result of membrane treatment of urine using a cellulose acetate semipermeable membrane and a polyacrylonitrile semipermeable membrane with a molecular weight cutoff of 20,000 to 40,000,
The processing time could be significantly shortened to 1/-1/4 compared to the case of the cellulose acetate semipermeable membrane having a molecular weight cut off of 4,000. However, the removal of the surfactant in urine was insufficient, and the separation of the urine-solvent interface was incomplete when the permeate was shaken with a solvent and then allowed to stand still for liquid separation. On the other hand, when urine is treated with a polysulfone semipermeable membrane having approximately the same molecular weight cutoff, the membrane treatment time is shortened, and at the same time surprisingly, surfactant substances are also retained on the membrane and the permeate is It was found that the liquid separation properties during solvent extraction were good and the recovery rate of the drug was quantitative.

The polysulfone semipermeable membrane used in the membrane treatment of the present invention is obtained by forming a membrane from a polymer represented by any of the structural formulas shown below.

The mechanism by which polysulfone semipermeable membranes block surfactants without allowing them to pass through is unknown, but polysulfone semipermeable membranes have more aromatic rings in their molecular chains than cellulose acetate membranes and polyacrylonitrile membranes. This is a highly hydrophobic polymer membrane, and it is thought that the hydrophobic skeleton portion in this molecular chain has a hydrophobic interaction with the lipophilic group portion of the surfactant in urine.

The inventors have also found that the separation of surfactant substances by this semipermeable membrane gives even better results when salts such as common salt are added to the urine to be tested.

The salts to be added are preferably halogenated alkali metal salts or halogenated earth metal salts. For example, common salt, potassium chloride, etc. can be used, and the amount thereof is 0.5 to 3% relative to the urine to be tested.
Approximately 0% is appropriate. It is thought that by adding these salts, the molecules of surface-active substances associate to form micelles, improving the separation efficiency.As a semipermeable membrane, not only polysulfone membranes but also cellulose acetate membranes and polyacrylic nitric membranes can be used. - The separation of surface-active substances can be considerably improved by the addition of salts even when using membranes.

That is, the present invention provides a rapid detection method in which urine to be tested is treated using a polysulfone semipermeable membrane with a molecular weight cutoff of 20,000 to 400,000, followed by solvent extraction and quantitative analysis of drugs extracted into the solvent. Therefore, it does not require any special pre-treatment and can be used as a conventional method.
This is a rapid detection method for drugs in urine, which is an analysis method that can quickly extract with a 15 to 10 times smaller amount of solvent and improve analysis speed and accuracy.

Further, the method for rapid detection of drugs in urine according to claim 1 is characterized in that a halogenated alkali metal salt or a halogenated alkaline earth metal salt is added to the urine to be tested and subjected to membrane treatment.

The present invention will be explained below with reference to Examples.

Example 1 and Comparative Example 1 A filtration device with stirring and pressure device (membrane area 31.2c4) shown in Utility Model Registration Application No. 57-95965 was used as a filtration device.
was used. A polysulfone semipermeable membrane or the like was used as the membrane.

6- 50 liters of urine to be tested was filtered using the above filtration device under nitrogen pressure (9/r, g 7 c, #) without stirring.

Although it is possible to add a solvent to the permeated urine to extract the drug and use it for analysis, we conducted a small-volume extraction test in a test tube to determine the effectiveness of membrane treatment in removing surfactants.

That is, 10ml of urine permeated through the membrane treatment was collected in a 20me test tube, 3g of common salt and 0.3ml of aqueous ammonia (28%) were added, and ether was further added as an extraction solvent.
Shake vigorously for 1 minute. The liquid suspended in the shaker is allowed to stand still, and the state of separation at the urine-solvent interface is observed after 2 minutes. If the separation is insufficient, add 1rnI of ether! Add
Perform the same operation and observe the liquid separation state again. Even in this case, if the liquid separation is still insufficient, add an additional 3 m7 of ether!
and perform extraction processing. In this case, the liquid separation state is determined when the suspended portion in the solvent layer is 1/10 of the amount of solvent added.
In the following cases, those with good separation, no suspended portion, and clear separation into a solvent layer and an aqueous layer were evaluated as excellent.

The test results according to the above method are shown in Table 1.

The drug in the illegally extracted organic solvent layer could then be subjected to appropriate concentration treatment and then quantitatively analyzed by gas chromatography or high-performance liquid chromatography.

Example 2 and Comparative Example 2 Urine from individuals different from those in Example 1 and Comparative Example 1 was used as test urine, and filtration and solvent extraction were performed in the same manner as in Example 1 and Comparative Example 1. The same treatment was also performed on urine to be tested to which 30 parts of common salt had been added. The results are shown in Table 2. The urine tested in this example had a lower surfactant content than that in Example 1, and was relatively easy to manipulate.
It was found that the separation property was further improved by adding salt.

Claims (2)

[Claims] (1) In the drug detection method in urine, which involves adding a solvent to urine, shaking it to separate the liquids, and then analyzing the drug in the solvent layer, the urine to be tested is first treated with a polysulfone semipermeable membrane and then shaken with a solvent. Characteristic rapid detection method for drugs in urine. (2) The method for rapid detection of drugs in urine according to claim 1, which comprises adding a halogenated alkali metal salt or a halogenated alkaline earth metal salt to the urine to be tested and subjecting it to membrane treatment.