JP2009150730A - Agitation determination method and analyzer - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an agitation determination method capable of certainly and easily determining adequacy of agitation, and to provide an analyzer. <P>SOLUTION: The agitation determination method is provided for the analyzer that analyzes a liquid sample by agitating the liquid sample reserved in a vessel and measuring an optical property of the reacted reactant liquid, and the analyzer is provided. The agitation determination method includes a light measurement step of measuring with time the optical property of a dilution determination solution of a dilution liquid and a determination liquid for determining agitation stirred within the vessel; and a determination step of determining as inferior agitation when the sum of absolute values of the measurement value differences of the dilution determination solution at two adjacent measurement points with time is above a predetermined reference value. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to a stirring determination method and an analysis apparatus.

  Conventionally, an analyzer for analyzing a biological sample such as blood or urine analyzes the component concentration of the biological sample by measuring the optical characteristics of the reaction solution obtained by reacting the specimen made of the biological sample with the reagent. . For this reason, in order for the analyzer to stir the specimen and the reagent sufficiently, the stirring apparatus that directly stirs the specimen and the reagent using a stirring rod (for example, refer to Patent Document 1) or using sound waves. Various stirring devices such as a stirring device that stirs a sample and a reagent in a non-contact manner are used.

JP 2003-57249 A

  By the way, when determining the quality of stirring by a stirrer, conventionally, a liquid sample immediately after stirring by inversion and the same liquid sample immediately after stirring by a stirrer are measured with a spectrophotometer, and the respective absorbances are compared. It was judged by. In this case, the measurement of the liquid sample is performed once both when stirring by overturning mixing and when stirring with a stirring device. For this reason, when stirring with a stirrer, the measured value is the same as the liquid sample stirred by overturning mixing, even though the stirring of the liquid sample is insufficient due to malfunction of the device, etc. There was a problem of being overlooked. In addition, both stirring by overturning mixing and stirring by a stirrer measure with a spectrophotometer other than the analyzer, so that there is a problem that the work of setting the liquid sample on the spectrophotometer becomes complicated. It was.

  This invention is made | formed in view of the above, Comprising: It aims at providing the stirring determination method and analyzer which can determine the quality of stirring reliably and simply.

  In order to solve the above-described problems and achieve the object, the stirring determination method of the present invention stirs a liquid sample held in a container and measures the optical characteristics of the reacted reaction solution. A method for determining the stirring of an analytical apparatus for analysis, comprising: a photometric step for measuring the optical characteristics of a dilution determination solution obtained by stirring the dilution solution and the determination solution for stirring determination in the container over time; And a determination step of determining a stirring failure when the sum of the absolute values of the differences between the measured values of the dilution determination solutions at two matching photometric points is equal to or greater than a preset reference value.

  In the stirring determination method of the present invention, in the above invention, the determination step determines that the stirring is poor when a value obtained by dividing the sum of the absolute values by the absorbance standard value is equal to or greater than a preset standard reference value. It is characterized by that.

  In the stirring determination method of the present invention, in the above invention, the two photometric points adjacent to each other over time are included in the final photometric point from the photometric point after stirring the dilution liquid and the determination liquid. It is characterized by.

  The stirring determination method of the present invention is characterized in that, in the above invention, the photometric step measures the optical characteristics in at least two liquid amounts having different amounts of the dilution determination solution.

  The stirring determination method of the present invention is characterized in that, in the above invention, the photometric step measures the optical characteristics over time when the stirring mode and the amount of the dilution determination solution are different. And

  In order to solve the above-described problems and achieve the object, the analyzer of the present invention stirs the liquid sample held in the container and measures the optical characteristics of the reacted reaction solution to measure the liquid sample. A photometric means for measuring the optical characteristics of the dilution determination solution obtained by stirring the dilution liquid and the determination liquid for stirring determination in the container over time; It is characterized in that there is provided a determination means for determining a stirring failure when the sum of absolute values of differences in the measured values of the dilution determination solution at a photometric point is equal to or greater than a preset reference value.

  Further, the analyzer according to the present invention is characterized in that, in the above invention, the determination means determines that the stirring is poor when a value obtained by dividing the sum of the absolute values by the standard value of absorbance is equal to or greater than a standard reference value. To do.

  In the case of a non-contact stirring type stirring device using a surface acoustic wave element, the stirring mode is a state in which the frequency at the time of stirring by the surface acoustic wave element is changed, and a contact stirring method using a stirring bar In the case of this stirring device, it means a state in which the size of the stirring rod, the number of revolutions, etc. are changed. The agitation mode is changed when the amount or type of liquid to be agitated is different or when the container is changed.

  The stirring determination method of the present invention includes a photometric step of measuring the optical characteristics of a dilution determination solution obtained by stirring a dilution solution and a determination solution for stirring determination in a container over time, and two photometric points adjacent to each other over time. A determination step of determining a stirring failure when the sum of the absolute values of the differences in the measured values of the dilution determination solution is equal to or greater than a preset reference value, and the analysis device of the present invention is a diluted solution dispensed in a container And the determination solution for stirring determination are determined to be poor stirring when the sum of absolute values of the difference between measured values at two adjacent photometric points over time is equal to or greater than a preset reference value. Since the means is provided, it is possible to reliably and easily determine whether the stirring is good or bad.

  Hereinafter, embodiments of the stirring determination method and the analysis apparatus according to the present invention will be described in detail with reference to the drawings. FIG. 1 is an automatic analyzer equipped with a non-contact stirring type stirring device as an analyzing device of the present invention, and is a diagram showing an overall configuration of a biochemical automatic analyzer that executes the stirring determination method of the present invention. . FIG. 2 is a perspective view showing a state in which the contact of the power transmission body is brought into contact with the electric terminal of the surface acoustic wave element attached to the cuvette. FIG. 3 is a side view showing the side surface of the cuvette of FIG. 2 together with the surface acoustic wave element.

  As shown in FIG. 1, the automatic analyzer 1 includes a rack supply device 2, a reaction unit 4, a first reagent cold storage 7 and a second reagent cold storage 8, an optical measurement unit 14, a control unit 16, and a first stirring device 21. And a second stirring device 25. In the automatic analyzer 1, the sample dispensing device 3 is provided between the rack supply device 2 and the reaction unit 4, and the first reagent dispensing device 5 is disposed between the reaction unit 4 and the first reagent cooler 7. However, a second reagent dispensing device 6 is provided between the reaction unit 4 and the second reagent cold storage 8 respectively.

  As shown in FIG. 1, the rack supply device 2 has a plurality of racks 2a arranged therein, and a sample cup 2b holding a sample is mounted on each rack 2a. The rack supply device 2 sequentially transports the rack 2a along the path indicated by the arrow, and the sample held in each sample cup 2b by the probe 3a of the sample dispensing device 3 is distributed to the cuvette (container) C of the reaction unit 4. Noted.

  Here, an STAT table (not shown) for an emergency sample is arranged in the vicinity of the sample dispensing apparatus 3, and a dye container holding a dye solution is set on the STAT table. Accordingly, the dye solution is dispensed from the dye container to the cuvette (container) C of the reaction unit 4 by the probe 3 a of the sample dispensing device 3. For example, when using a dye solution as a determination solution used for stirring determination, the diluent is an acid solvent obtained by diluting hydrochloric acid, sulfuric acid, or the like with ion-exchanged water using the dye solution used, or ion-exchanged water. In some cases, the alkaline solvent diluted in (1) is used as a diluent, and the hydrogen ion concentration (pH) of the diluent is selected according to the dye solution to be used.

  Further, the amount of the dye solution dispensed by the sample dispensing device 3 when executing the stirring determination method of the present invention is arbitrary, but the first reagent dispensing device 5 and the second reagent dispensing device 6 dispense. The amount of dilution water to be diluted is the total amount of the dye solution and the dilution water dispensed by the first reagent dispensing device 5 is close to the photometric minimum solution amount, and further diluted by the second reagent dispensing device 6 Set so that the total amount of water added is the maximum amount of sample that can be measured. For example, when the amount of the photometric solution in the cuvette C is 150 to 400 μL, the amount of the dye solution dispensed by the sample dispensing device 3 is 1 μL, and the amount of the diluted water dispensed by the first reagent dispensing device 5 is 150 μL. The amount of dilution water dispensed by the second reagent dispensing device 6 is set to 250 μL.

  As shown in FIG. 1, the reaction unit 4 includes a heat retaining member 4a and a cuvette wheel (not shown). The heat retaining member 4a is arranged inside and outside in the radial direction of the cuvette wheel, and a photometric opening 4c is formed at a position corresponding to the optical measuring unit 14. The cuvette wheel rotates while holding a plurality of cuvettes C at a temperature around the body temperature, for example, rotates in one cycle clockwise (1 turn-1 cuvette) / 4 minutes, and in 4 cycles, it rotates one cuvette clockwise. Rotate.

  Since the first reagent cool box 7 and the second reagent cool box 8 have the same configuration, the first reagent cool box 7 will be described, and the second reagent cool box 8 will be described in detail with reference numerals corresponding to the corresponding components. The detailed explanation is omitted.

  As shown in FIG. 1, the first reagent cool box 7 is provided with a plurality of reagent bottles 7a holding the first reagent and a dilution water bottle 7b holding dilution water composed of ion-exchanged water. A predetermined reagent or dilution water is dispensed into the cuvette C by the probe 5 a of the apparatus 5. Each of the plurality of reagent bottles 7a is filled with a predetermined reagent corresponding to an inspection item, and an information recording medium (not shown) such as a barcode label for displaying information on the stored reagent is attached to the outer surface. At this time, an information recording medium (not shown) is also attached to the outer surface of the dilution water bottle 7b. In the cuvette C into which the first reagent has been dispensed, the sample and the first reagent are stirred by the first stirring device 21. A reading device 9 that reads information from the information recording medium affixed to each reagent bottle 7 a and dilution water bottle 7 b and outputs the information to the control unit 16 is installed on the outer periphery of the first reagent cooler 7. The reading device 10 reads information from the information recording medium attached to each reagent bottle 8a and dilution water bottle 8b in the second reagent cooler 8.

  As shown in FIG. 1, the optical measurement unit 14 includes a light source 14a and a photometric sensor 14b. The light source 14a emits analysis light for analyzing the reaction solution in the cuvette C in which the reagent and the sample have reacted. The photometric sensor 14b measures the luminous flux emitted from the light source 14a and transmitted through the opening 4c and the reaction solution or diluted dye solution in the cuvette C. The cuvette C in which the reaction solution and the diluted dye solution are photometrically measured in this manner is discarded by the cleaning / drying unit 15 with the reaction solution and the diluted dye solution being sucked therein, and the wash water supplied from the wash water tank. After the inside is cleaned by the above, it is dried by blowing pressurized air. In the cuvette C, a new sample is again dispensed by the probe 3a of the sample dispensing device 3 and used for analysis.

  As the control unit 16, for example, a microcomputer having a storage function for storing the analysis result is used, and the photometric sensor 14b, the bar code label readers 9 and 10, the analysis unit 16a, the input unit 17, the display unit 18, the first The first stirrer 21 and the second stirrer 25 are connected. The control unit 16 controls the operation of each unit of the automatic analyzer 1 and regulates the analysis work when the reagent lot or expiration date is out of the installation range based on the information read from the information recording medium. The automatic analyzer 1 is controlled or a warning is issued to the operator. More specifically, the control unit 16 includes an analysis unit 16a and a determination unit 16b.

  The analysis unit 16a analyzes and stores the component concentration of the specimen from the absorbance (optical characteristics) of the reaction liquid of the specimen and the reagent in the cuvette C based on the light quantity signal measured by the photometric sensor 14b. The determination unit 16b determines the quality of stirring based on the absorbance measured for the diluted dye solution in the cuvette C.

  The input unit 17 is a part that performs an operation of inputting the number of samples, examination items, and the like to the control unit 16, and for example, a keyboard or a mouse is used. The display unit 18 displays an analysis content including the analysis result, an alarm including the quality of stirring, and a display panel or the like is used.

  The first stirrer 21 and the second stirrer 25 stir the sample and reagent dispensed in the cuvette C in a non-contact manner by means of sound waves, react them, and dispense them to the cuvette C when judging the quality of the agitation. Stir the dye solution and / or diluted water. In order to perform this non-contact stirring, the heat retaining member 4 a of the reaction unit 4 is open at a portion facing the first stirring device 21 and the second stirring device 25. The cuvette C is set on the cuvette wheel with the surface acoustic wave element 24 attached to the side wall facing outward.

  The operation of the first stirring device 21 and the second stirring device 25 is controlled by the control unit 16 and the configuration is the same, so the first stirring device 21 will be described, and the second stirring device 25 has the same reference numerals for the same components. The description is omitted by attaching.

  The 1st stirring apparatus 21 has the power transmission body 22, the positioning member 23, and the surface acoustic wave element 24, as shown in FIGS.

  As shown in FIG. 1, the power transmission body 22 is disposed in a position facing the cuvette C in the horizontal direction at positions facing each other on the outer periphery of the reaction unit 4, and is supplied from a high-frequency AC power source of several MHz to several hundred MHz Is transmitted to the surface acoustic wave element 24. The power transmission body 22 includes a drive circuit and a controller, and has a brush-like contact 22a that abuts on the electrical terminal 24c of the surface acoustic wave element 24 as shown in FIG. And as shown in FIG. 1, the power transmission body 22 is supported by the positioning member 23, and transmits electric power from the contact 22a to the electrical terminal 24c when the rotation of the cuvette wheel stops.

  The operation of the positioning member 23 is controlled by the control unit 16, and during power transmission in which power is transmitted from the power transmission body 22 to the electrical terminal 24c, the power transmission body 22 is moved to move around the reaction unit 4 between the power transmission body 22 and the electrical terminal 24c. For adjusting the relative arrangement in the direction and the radial direction, for example, a two-axis stage is used. Specifically, the positioning member 23 stops its operation while the reaction unit 4 rotates, and holds the power transmission body 22 and the electric terminal 24c at a constant distance. And when the reaction table 4 stops, the positioning member 23 will operate | move under control of the control part 16, will move the power transmission body 22, and will adjust a position so that the power transmission body 22 and the electrical terminal 24c may oppose. At the same time, the positioning member 23 transmits power from the power transmitting body 22 to the electric terminal 24c by driving the surface acoustic wave element 24 by bringing the contact 22a and the electric terminal 24c into contact with each other under the control of the control unit 16. To do.

  The surface acoustic wave element 24 is attached to the side wall of the cuvette C, and as shown in FIG. 3, a vibrator 24b made of a comb electrode (IDT) is provided on the surface of the substrate 24a. The vibrator 24b is a sound wave generating unit that converts electric power transmitted from the power transmitting body 22 into surface acoustic waves (ultrasonic waves). The vibrator 24b is connected to an electrical terminal 24c serving as a power receiving means by a conductor circuit 24d. The surface acoustic wave element 24 is attached to the side wall of the cuvette C via the acoustic matching layer with the vibrator 24b, the electric terminal 24c, and the conductor circuit 24d facing outward.

  The automatic analyzer 1 configured as described above operates under the control of the control unit 16 and dispenses the first reagent to each of the plurality of cuvettes C that are conveyed along the circumferential direction by the rotating cuvette wheel. After the first reagent is sequentially dispensed by the apparatus 5, the specimen is sequentially dispensed from the plurality of specimen containers 2 b held in the rack 2 a by the specimen dispensing apparatus 3. The second reagent is sequentially dispensed from the reagent container 3a by the second reagent dispensing device 6 into the cuvette C into which the specimen has been dispensed.

  During this time, the cuvette C into which the reagent or sample has been dispensed is optically measured when the reagent or sample is stirred by the first stirring device 21 or the second stirring device 25 each time the cuvette wheel stops and the cuvette wheel rotates again. Pass through part 14. At this time, the reaction liquid in which the reagent in the cuvette C has reacted with the sample is measured for optical characteristics by the optical measurement unit 14, and the component concentration is determined by the control unit 16 based on the optical signal input from the optical measurement unit 14. Etc. are analyzed. Then, the cuvette C for which the measurement of the reaction solution has been completed is transferred to the washing unit 15 and washed, and then used again for analyzing the specimen.

  At this time, the automatic analyzer 1 determines the quality of stirring in each cuvette in advance by, for example, executing the stirring determination method of the present invention before starting the analysis. Hereinafter, the determination procedure of the present invention will be described with reference to FIG.

  First, when execution of agitation determination is input from the input unit 17 to the control unit 16, the control unit 16 firstly dispenses a predetermined amount (for example, 150 μL) of dilution water from the dilution water bottle 7b to the cuvette C. A command signal is output to one reagent dispensing device 5. As a result, the probe 5a dispenses a predetermined amount of dilution water W into the cuvette C as shown in FIG.

  Next, the control unit 16 outputs a command signal to the first stirring device 21 to stir (MIX0) the dilution water W dispensed in the cuvette C, and then outputs a command signal to the optical measurement unit 14. As shown in FIG. 4, the absorbance A0 (background) of the cuvette C holding the dilution water W is measured. Next, the control unit 16 outputs a command signal to the sample dispensing device 3 so as to dispense a predetermined amount (for example, 1 μL) of the dye solution from the dye container of the STAT table to the cuvette C. As a result, the probe 3a dispenses a predetermined amount of the dye liquid Lp into the cuvette C as shown in FIG. Here, as the dye solution, an orange G solution (manufactured by Wako Pure Chemical Industries, Ltd.) having an absorbance of about 200 diluted with water was used.

  Thereafter, the control unit 16 outputs a command signal to the first stirring device 21 to stir (MIX1) the diluted water W and the dye solution Lp dispensed in the cuvette C, and dilute as shown in FIG. The dye solution is Lp1. Thereafter, the control unit 16 outputs a command signal to the optical measurement unit 14 to measure the absorbance A1 of the cuvette C holding the diluted dye solution Lp1. Next, the control unit 16 outputs a command signal to the second reagent dispensing device 6 so as to dispense a predetermined amount (for example, 250 μL) of diluted water from the diluted water bottle 8b to the cuvette C. As a result, the probe 6a dispenses a predetermined amount of dilution water W into the cuvette C as shown in FIG.

  Next, the control unit 16 outputs a command signal to the second stirrer 25 to stir (MIX2) the diluted water W and the diluted dye solution Lp1 dispensed in the cuvette C, and dilute as shown in FIG. The dye solution is Lp2. Thereafter, the control unit 16 outputs a command signal to the optical measurement unit 14 to measure the absorbance A2 of the cuvette C holding the diluted dye solution Lp2. After measuring the absorbances A0 to A2 in this way, the controller 16 subtracts the absorbance A0 as the background from the measured absorbances A1 and A2 of the cuvette C to obtain only the diluted dye solutions Lp1 and Lp2 having different concentrations. The value is the corrected absorbance. This calculation is performed by the determination unit 16b.

  At this time, in the automatic analyzer 1, the cuvette wheel rotates while holding the plurality of cuvettes C. For example, the cuvette wheel rotates in the clockwise direction (1 turn-1 cuvette) / 4 minutes in one cycle. The above-described absorbance measurement is performed in parallel. Here, as shown in FIG. 5, the absorbance is measured at a total of 28 photometric points (P0 to P27) over time per cuvette C including the photometry of the absorbance A0. At this time, when the cuvette C to be used is not contaminated and ion exchange water or pure water is used as dilution water, the absorption of the analysis light is very small and the measurement of the optical characteristics can be omitted. It is not always necessary to perform photometry. However, when the above-mentioned acid solvent or alkaline solvent is used as the diluent, the analysis light is absorbed by the diluted water. Therefore, in order to accurately measure the optical characteristics and judge the quality of the stirring, the absorbance A0 is used. It is preferable to perform photometry.

  FIG. 5 shows an example of measurement of absorbance when the diluted water dispensed in the cuvette C and the dye solution (orange G solution) are well stirred and the judgment unit 16b judges that the stirring is good. Show. In FIG. 5, TM1 indicates the timing when the diluted water W and the dye solution Lp dispensed in the cuvette C are stirred (MIX1) to obtain the diluted dye solution Lp1, and TM2 is re-dispensed with the stirred diluted dye solution Lp1. The timing of stirring (MIX2) the diluted water W to obtain a diluted dye solution Lp2 is shown, and specifically corresponds to the photometric points P0 to P1 and the photometric points P11 to P12.

  Next, based on the absorbance of all the cuvettes C thus measured, the determination unit 16b corrects the corrected absorbances XH2 to XH11 and XL13 to XH27 at the photometric points P2 to P11 and P13 to P27 for each cuvette C. Is calculated. The corrected absorbances XH2 to XH11 of the photometric points P2 to P11 are obtained, for example, by subtracting the absorbance (A0) of the photometric point P0 as the background from the absorbance (A2) of the photometric point P2 for the photometric point P2. Similarly, the corrected absorbances XL13 to XH27 of the photometric points P13 to P27 are also obtained by subtracting the absorbance (A0) of the photometric point P0 as the background from the absorbance (A13) of the photometric point P12, for example. Ask for.

Then, the determination unit 16b calculates the absolute value of the difference between the corrected absorbances XH2 to XH11 and XL13 to XH27 at two adjacent photometry points based on the corrected absorbances XH2 to XH11 and XL13 to XH27 calculated for each cuvette C. The sums DH and DL are calculated. Here, sums DH and DL of absolute values are given by the following equations. Also, absorbance reference values VH and VH are set in advance based on the absorbance measured for each concentration of the dilution determination solution to be used, and input from the input unit 17 to the determination unit 16b. However, the reference values VH and VL are set empirically and experimentally based on the dilution determination solution used.
DH = {| XH2-XH3 | + | XH3-XH4 | + ......... + | XH9-XH10 | + | XH10-XH11 |}
DL = {| XL13-XL14 | + | XL14-XL15 | + ...... + | XL25-XL26 | + | XL26-XL27 |}

  The determination unit 16b determines the quality of stirring for each cuvette C based on the absolute value sums DH and DL and the absorbance reference values VH and VL thus calculated. At this time, the determination unit 16b determines that the stirring is good when the sum of the absolute values is DH <VH or DL <VL with respect to the absorbance reference value, and the sum of the absolute values is DH with respect to the absorbance reference value. When ≧ VH or DL ≧ VL, it is determined that the stirring is poor.

  Here, the dilution dispensed in the cuvette C is not performed when the stirring of the dilution water W and the dye liquid Lp dispensed in the cuvette C (MIX1) and the stirring of the dilution water W and the dye solution Lp1 (MIX2) are not performed. An example of the measurement of absorbance when the water W and the dye liquid Lp are stirred (MIX1) but not the diluted water W and the diluted dye solution Lp1 (MIX2) is shown in FIG. FIG. 6 shows an example of absorbance measurement in the case of MIX2). Further, among the measurement examples of absorbance shown in FIG. 6, an enlarged measurement example of absorbance at photometric points P0 to P11 is shown in FIG. 7, and an enlarged measurement example of absorbance at photometric points P12 to P27 is shown in FIG. Shown in

  At this time, the determination procedure performed by the determination unit 16b for each cuvette C will be described with reference to the flowchart shown in FIG.

  First, the determination unit 16b determines that the sum DH of the absolute values of the differences in the corrected absorbance at two adjacent photometric points of the cuvette C holding the diluted dye solution Lp1 is smaller than the absorbance reference value VH (DH <VH). ) Is determined (step S100). When the determination result is negative (step S100, No), the cuvette C holding the diluted dye solution Lp1 has the sum DH of absolute values equal to or higher than the reference value VH, and the stirring is poor. For this reason, the determination part 16b outputs a command signal to the display part 18 so that the identification number of the cuvette C is displayed as an error (step S102).

  On the other hand, when the determination result is affirmative (step S100, Yes), the cuvette C holding the diluted dye solution Lp1 has a sum DH of absolute values smaller than the reference value VH and is well stirred. Therefore, the determination unit 16b determines that the sum DL of the absolute values of the differences in the corrected absorbance at two adjacent photometric points of the cuvette C holding the diluted dye solution Lp2 is smaller than the absorbance reference value VL (DL < VL) or not (step S104).

  When the determination result is negative (step S104, No), the cuvette C holding the diluted dye solution Lp2 has a sum of absolute values DL equal to or greater than the absorbance reference value VL, and the stirring is poor. Therefore, the determination unit 16b outputs a command signal to the display unit 18 so that the identification number of the cuvette C is displayed as an error (step S102).

  On the other hand, if the determination result is affirmative (step S104, Yes), the cuvette C holding the diluted dye solution Lp2 has a sum of absolute values DL smaller than the absorbance reference value VL, and is well stirred. The determination unit 16b determines whether or not the sums DL and DL of the absolute values of the individual cuvettes C are smaller than the absorbance reference values VH and VL, and then ends the determination.

  Here, the stirring determination method of the present invention determines the quality of stirring based on a common measure of absorbance, but the diluted dye solution Lp1 and the diluted dye solution Lp2 are apparent from the corrected absorbance values. The concentration is different. For this reason, if the absorbance of the diluted dye solution Lp1 and the absorbance of the diluted dye solution Lp2 having different concentrations are handled in common, an error may occur in the determination of the quality of stirring.

Therefore, even in a diluted dye solution obtained by diluting the same dye solution, when determining the quality of stirring using the absorbance of diluted dye solutions having different concentrations, the absolute value is The standard absorbance ratios DNH and DNL normalized by dividing the sum DH and DL by the absorbance standard values NH and NL are compared with preset standard reference values VNH and VNL to determine the quality of stirring.
DNH = {| XH2-XH3 | + | XH3-XH4 | +
+ | XH9−XH10 | + | XH10−XH11 |} / NH × 100 (%)
DNL = {| XL13-XL14 | + | XL14-XL15 | +
+ | XL25-XL26 | + | XL26-XL27 |} / NL × 100 (%)

  In this case, as the absorbance standard values NH and NL, for example, the absorbance of the dilution determination solution at the final photometric point P27, the average absorbance of all the cuvettes C measured at the same concentration, or the concentration of the dilution determination solution The absorbance value determined in advance based on the above is used. The standard reference values VNH and VNL are, for example, 1%. That is, the determination unit 16b is set so that when the calculated values of the standard absorbance ratios DNH and DNL are 1% or more, it is determined that the stirring is poor, and when it is smaller than 1%, it is determined that the stirring is good. However, the standard reference values VNH and VNL are empirically set experimentally based on the dye solution to be used, and thus the determination solution, as in the case of the reference values VH and VL.

  Thus, when the standard absorbance ratios DNH and DNL obtained by dividing the sum of absolute values DH and DL by the standard values NH and NL are used, even if the concentration of the diluted dye solution is different, the change in absorbance is observed. The variation of the sum DH and DL of the absolute values due to is suppressed to be small. As a result, the absorbance of the diluted dye solution Lp1 and the absorbance of the diluted dye solution Lp2 having greatly different concentrations can be handled in common when determining the quality of stirring.

  As is clear from the above description, according to the stirring determination method and the automatic analyzer 1 of the present invention, the sum of the absolute values of the differences between the measured values of the optical characteristics at two photometric points adjacent to each other over time of the cuvette C. Is compared with a preset reference value to determine whether the stirring is good or bad. For this reason, since the stirring determination method and the automatic analyzer 1 of the present invention can use the optical measuring unit 14 that is inherently mounted on the automatic analyzer 1, the quality of stirring can be reliably and easily determined. Can be determined.

  In the above-described stirring determination method, the quality of stirring may be determined by comparing the difference in absorbance at two measurement points adjacent to each other over time with a preset reference value.

Further, instead of the standard absorbance ratios DNH and DNL, the fluctuation absorbance ratios DYH and DYL represented by the following formulas may be compared with preset standard reference values VYH and VYL to determine whether or not the stirring is good.
DYH = (XHmax−XHmin) / XH11 × 100 (%)
DYL = (XLmax−XLmin) / XL27 × 100 (%)

  In the above formula, XHmax and XHmin are the maximum value and the minimum value of the corrected absorbances XH2 to XH11 at the photometric points P2 to P11. XLmax and XLmin are the maximum and minimum values of the corrected absorbances XL13 to XH27 at the photometric points P13 to P27. In this case, the standard reference values VYH and VYL are set in the same manner as the standard reference values VNH and VNL, for example, 1%. That is, the determination unit 16b is set so that when the calculated values of the fluctuation absorbance ratios DYH and DYL are 1% or more, it is determined that the stirring is poor, and when it is smaller than 1%, the stirring is determined to be good.

  Here, although the above-mentioned embodiment demonstrated the automatic analyzer equipped with the non-contact stirring-type stirring apparatus, the stirring determination method and analyzer of this invention use a stirring bar, as shown in FIG. The present invention can also be applied to the automatic analyzer 20 equipped with a contact stirrer.

  In the automatic analyzer 20, instead of the first stirrer 21 and the second stirrer 25, the first stirrer 11 and the second stirrer 12 of the contact stirrer type are disposed, and the surface acoustic wave element 24 is disposed in the cuvette C. It is not installed. Here, the stirring device 11 is normally used for stirring the first reagent and the specimen, and the stirring device 12 is used for stirring when the second reagent is further dispensed. That is, the first stirrer 11 and the second stirrer 12 stir the specimen or reagent dispensed in the cuvette C with the stirring bars 11a and 11b or the stirring bar 12a. When determining the quality of stirring, the stirring bar 11a is used for stirring the dilution water (MIX0), and the stirring bar 11b is used for stirring the cleaning water and the dye solution (MIX1). The stirring rod 12a is used for stirring the cleaning water and the diluted dye solution (MIX2).

  Here, the cuvette C used in the automatic analyzer 1 has a surface acoustic wave element 24 attached to each cuvette. For this reason, the stirring performance of the first stirring device 21 and the second stirring device 25 of the non-contact stirring method differs for each cuvette C. Accordingly, the automatic analyzer 1 equipped with the first stirrer 21 and the second stirrer 25 needs to determine whether or not the stirring is good for all the cuvettes C.

  On the other hand, since the 1st stirring apparatus 11 and the 2nd stirring apparatus 12 are mechanical stirring apparatuses using a stirring rod, even if cuvette C differs, stirring performance does not change a lot. Therefore, the automatic analyzer 20 equipped with the first stirrer 11 and the second stirrer 12 can measure the optical characteristics of the diluted determination solution after stirring for some cuvettes C, for example, five cuvettes. Good. For some of the cuvettes C measured, the quality of stirring is determined based on the sum DH, DL of absolute values and the reference values VH, VL of absorbance obtained as described above.

  However, the automatic analyzer 1 equipped with the non-contact stirring type first stirring device 21 and the second stirring device 25 applies the stirring determination method of the present invention to the cuvette wheel without taking out the cuvette C from the cuvette wheel. There is an advantage that the quality of stirring can be easily determined as part of the analysis work for each cuvette C with the cuvette C set.

  In the above stirring determination method, the quality of stirring was determined based on the measured absorbance when the diluted dye solutions Lp1 and Lp2 having different concentrations were measured. When either one of the diluted dye solutions was measured, The quality of stirring may be judged based on the measured value of the absorbance of, or three or more diluted dye solutions having different concentrations may be used. At this time, as shown in FIG. 4, the automatic analyzer 1 changes the stirring mode such as the driving frequency and driving power for driving the surface acoustic wave element 24 for each stirring (MIX0 to MIX2) having different liquid amounts. The automatic analyzer 20 may replace the stirring bars of the first stirring device 11 and the second stirring device 12 according to the amount of liquid to be stirred.

  In addition, the determination liquid for stirring determination can be diluted with a diluent, and if the optical characteristics can be measured, a calibrator or the like that conforms to the sample can be used instead of the dye liquid. Good.

  When displaying an error, the determination unit 16b adds a remark to that effect to the measurement value, and in the case of the automatic analyzer 1, the determination unit 16b does not use the cuvette C with the identification number displayed in the error in subsequent analysis work. It may be displayed that the cuvette C should be replaced together with an error display. On the other hand, in the case of the automatic analyzer 20, the determination unit 16b adds a remark to that effect to the measurement value, and replaces the stirring rods of the first stirring device 11 and the second stirring device 12 that have failed to stir. A message to the effect is displayed.

  Moreover, although the dilution water was hold | maintained at the dilution water bottles 7b and 8b, and it has arrange | positioned in the 1st reagent cold storage 7 or the 2nd reagent cold storage 8, the 1st reagent dispensing apparatus 5 and the 2nd reagent dispensing apparatus 6 of FIG. You may use the ion exchange water for washing | cleaning discharged from the probes 5a and 6a.

  In addition, the measurement value and the reference value of the optical characteristics when stirring is appropriately performed for the dye solution having a predetermined dilution rate are stored in advance as reference data in the control unit, and the determination liquid and the dilution liquid for stirring determination The quality of the agitation may be determined by comparing the sum of absolute values of the differences in measured values of the optical characteristics of the dilution determination solution obtained by stirring with a reference value.

It is a figure which shows the whole structure of the automatic analyzer which mounts the stirring apparatus of a non-contact stirring system as an analyzer of this invention. It is a perspective view which shows the state which contacted the electrical contact of the surface acoustic wave element with which the contactor of the power transmission body was attached to the cuvette. It is a side view which shows the side surface of the cuvette of FIG. 2 with a surface acoustic wave element. It is a figure explaining the procedure which adjusts two types of dilution determination solutions by diluting the determination liquid for stirring determination with dilution water. It is a figure which shows an example of the measurement example of the light absorbency when stirring with the dilution water and the pigment | dye solution dispensed to the cuvette is performed favorably, and it determines with a determination part being good. It is a figure which shows the measurement example of the light absorbency when not stirring with the measurement example of the light absorbency when stirring shown in FIG. It is the figure which expanded the measurement example of the light absorbency of photometry point P0-P11 among the measurement examples of the light absorbency shown in FIG. It is the figure which expanded the measurement example of the light absorbency of the photometry point P12-P27 among the measurement examples of the light absorbency shown in FIG. It is a flowchart which shows the determination procedure which a determination part performs. FIG. 1 is a diagram showing an overall configuration of a biochemical automatic analyzer that performs an agitation determination method according to the present invention, which is an automatic analyzer equipped with a contact agitation type agitation device using a stirring rod as an analyzer of the present invention. .

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Automatic analyzer 2 Rack supply device 3 Sample dispensing device 4 Reaction part 5 First reagent dispensing device 6 Second reagent dispensing device 7 First reagent cold storage 8 Second reagent cold storage 9,10 Reader 11 First Stirrer 12 Second stirrer 14 Optical measurement unit 15 Cleaning / drying unit 16 Control unit 16b Determination unit 17 Input unit 18 Display unit 20 Automatic analyzer 21 First stirrer 25 Second stirrer 22 Power transmission unit 23 Positioning member 24 Surface Elastic wave element C cuvette

Claims (7)

A stirring determination method for an analyzer that stirs a liquid sample held in a container and analyzes the liquid sample by measuring optical characteristics of the reacted reaction solution,
A photometric step of measuring the optical characteristics of the dilution determination solution obtained by stirring the dilution liquid and the determination liquid for stirring determination in the container over time;
A determination step of determining a stirring failure when the sum of absolute values of differences between measured values of the dilution determination solution at two photometric points adjacent to each other over time is equal to or greater than a preset reference value;
The stirring determination method characterized by including.   2. The stirring determination method according to claim 1, wherein the determination step determines a stirring failure when a value obtained by dividing the sum of the absolute values by a standard value of absorbance is equal to or greater than a preset standard reference value.   The stirring determination method according to claim 1, wherein the two photometric points adjacent to each other with time are included in a final photometric point from a photometric point after stirring the dilution liquid and the determination liquid. .   The stirring determination method according to claim 3, wherein the photometric step measures the optical characteristics in at least two liquid amounts having different amounts of the dilution determination solution.   5. The stirring determination method according to claim 4, wherein the photometric step measures the optical characteristics over time when stirring is performed in a state where the stirring mode and the amount of the dilution determination solution are different. An analyzer for analyzing the liquid sample by stirring the liquid sample held in the container and measuring the optical characteristics of the reacted reaction solution,
Photometric means for measuring the optical characteristics of the dilution determination solution obtained by stirring the dilution liquid and the determination liquid for stirring determination in the container over time;
An analysis characterized by comprising a determination means for determining a stirring failure when the sum of absolute values of differences between measured values of the dilution determination solution at two adjacent photometric points over time is equal to or greater than a preset reference value. apparatus.   The analyzer according to claim 6, wherein the determination unit determines that the stirring is poor when a value obtained by dividing the sum of the absolute values by a standard value of absorbance is equal to or greater than a standard reference value.

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