JP2701734B2 - Adhesion residue evaluation method and device - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for evaluating adhered residues for confirming that there is no adhered residue after washing medical and food manufacturing facilities, and an adhered residue suitable for carrying out the method. It relates to an evaluation device.

[0002]

2. Description of the Related Art For example, in a pharmaceutical manufacturing process,
When manufacturing different types of drugs using a common manufacturing facility, the contamination of the next drug with the residues of the previously manufactured drug, especially biologically active substances, can cause serious accidents that can be life-threatening. Maybe. A method called a swab method is known as one of the evaluation methods for confirming the adhesion of the residue after washing of such a pharmaceutical manufacturing facility. This is done by wiping a fixed area (usually 10 × 10 cm) of the manufacturing equipment that has been washed with a material such as cotton or gauze, and dissolving and extracting it in a fixed amount of water or an organic solvent in order to collect measurement components from it. In this method, the target component in the extract is measured by means such as a liquid chromatograph, a gas chromatograph, a thin-layer chromatograph, and an infrared spectrophotometer.

[0003]

In the conventional swab method, after a wiping operation of a certain area of a manufacturing facility, a target component must be extracted and quantitatively fractionated. There is a problem that it takes time and effort in the process of analyzing components by liquid chromatography or the like.

Further, since the target component is determined and the component is analyzed, information on the target component can be obtained. However, if the production equipment is contaminated with other unpredictable components, it cannot be dealt with. There is a problem in that there is contamination by outside components, and even if this cleaning is insufficient, it is ignored.

In view of the above problems, the present invention quickly and easily reduces the measurement time and labor after a wiping operation when evaluating and judging components still remaining after washing of a pharmaceutical manufacturing facility or the like by a swab method. It is an object of the present invention to provide an attached residue evaluation method and an attached residue evaluation device suitable for carrying out the method.

[0006]

In order to achieve the above object, in the method for evaluating the adhesion residue according to the present invention, a fiber made of an inorganic material containing no carbon is used for a support made of an inorganic material containing no carbon. The adhered residue is collected by the fixed wiping device, and the wiping device is burned and oxidized in a carrier gas containing oxygen to convert the carbon content of the adhered residue into carbon dioxide. The amount of carbon in the material is determined, and the adhered residue is evaluated and determined.

Further, in the adhesion residue evaluation apparatus of the present invention, a sample boat on which a sample is placed is introduced into a heating furnace, and the sample is burned and oxidized in a carrier gas containing oxygen to convert carbon in the sample into carbon dioxide. This is a device that conducts this carbon dioxide together with a carrier gas to a gas analyzer and measures the same. A wiping device in which carbon-free inorganic material fibers are fixed to a support made of carbon-free inorganic material The sample boat is provided with a support portion for detachably supporting the sample boat, and the adhesion residue evaluation method of the present invention is implemented.

In the wiping device, carbon analysis is usually performed at a temperature of about 900 ° C., so that it can withstand this temperature and can be made of quartz glass, ceramic, metal, or the like having a hollow or rod-like shape. A quartz glass fiber or a ceramic fiber or a cloth, a plate, or a bulk is formed on a holding member having a plate shape or the like and fixed by a method such as welding, bonding, or clamping.

[0009]

According to the method and the apparatus for evaluating the adhesion residue, a certain area of the manufacturing equipment is wiped by the wiping device, and the wiping device is used as it is as a support for the sample boat (see FIG. 4).
Is set to At this time, as shown in FIG. 2, the wiping device has a structure in which ceramic fibers or the like are fixed to a hollow holder, and a handle is used which sandwiches and holds both ends of the wiping device from the left and right as shown in FIG. It is convenient and convenient for the wiping operation and the setting of the measuring device in the sample boat.

The wiping device set on the support portion of the sample boat is introduced into a heating furnace by operating a sample introduction rod, and the adhered residue wiped in the heating furnace is burned and oxidized in a carrier gas containing oxygen. As a result, the carbon content in the adhered residue is converted into carbon dioxide. The converted carbon dioxide is guided to a gas analyzer such as a non-dispersive infrared gas analyzer together with a carrier gas, and the residual carbon is measured and evaluated as the total amount of organic substances by the carbon analysis.

[0011] Therefore, since the entire amount of the adhered residue wiped off by the wiping device is used for the measurement, measurement with high sensitivity (1 µg or more) is possible. The combustion residue (oxidation reaction) removes the adhered residue that has been wiped off. As a result, the residue is washed, and after the measurement, it can be used again for wiping the next adhered residue.

[0012]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Referring to the drawings, an embodiment of an apparatus for carrying out the method for evaluating the adhesion residue of the present invention will be described. In FIG. 1, a quartz glass combustion tube 6 is provided inside a heating furnace 7 having a heating element 8. Is connected to a sample port block 5 having a support gas / carrier gas inlet 2 and a sample port cover 3 for inserting and removing a wiping device 10 as a sample.

The wiping device 10 is, as shown in FIG.
Since the carbon analysis is usually performed at a temperature of about 900 ° C., a hollow support 10 a made of an inorganic material such as quartz glass or ceramic that can withstand this temperature and does not contain carbon is also provided with carbon. Is formed by winding and fixing a heat-resistant inorganic quartz glass fiber or ceramic fiber 10b containing no. Such a wiping device 10
Is stored in a storage case (not shown) or the like until a predetermined area of a manufacturing facility (not shown) is wiped off and then used for measurement for evaluation and determination.

The wiping device 10 is mounted on the support portion 12 (see FIG. 4) of the sample boat 4 with the sample port cover 3 openable and closable. After the sample port cover 3 is closed, the operation of the sample introduction rod 1 is performed. By moving the sample boat 4 through the combustion tube 6 to the heating furnace 7 heated to a temperature of about 900 ° C., oxygen or purified air (0.1 to 1 liter) is used as a supporting gas and a carrier gas. / Min) is flowing, the combustion oxidation reaction is performed.

The rear half of the combustion tube 6 is filled with an oxidation catalyst 9 such as platinum, cobalt oxide, or copper oxide. In the combustion tube 6, organic substances in the residue adhering to the wiping device 10 evaporate. After being decomposed, it reaches the oxidation catalyst layer 9 together with the carrier gas. Under the action of the catalyst, all gas components are oxidized to carbon dioxide gas.

Outlet (carrier gas outlet) 11 of combustion tube 6
Denotes a gas processing unit 17 such as a drain separator (not shown).
Is connected to a non-dispersive infrared gas analyzer (NDIR) 13 capable of measuring carbon dioxide with high accuracy and high sensitivity without interference of other components, and contains carbon dioxide gas from the combustion tube 6. The carrier gas is guided to the NDIR 13 and the carbon content in the adhered residue wiped off by the wiping device 10 is measured. The NDIR 13 is calibrated in advance with a standard substance such as glucose, and the total amount of organic substances (carbon concentration) in the adhered residue in the data processing unit 14
Is calculated and displayed on the display unit 15 such as a CRT as a result of evaluation of the attached residue.

In this example, in an experiment using glucose, the quantification of 1 μg C could be measured with an accuracy of CV of 10% or less. Usually, the swab method uses 10 × 1 as an organic substance.
It is tested on the basis of 100 μg in a 0 cm wiping test.
(50% is the most common), so that the method of the present invention can sufficiently measure the time, and the time required for one hour or more in the conventional method can be measured in only 5 to 10 minutes.

As shown in FIG. 3, the wiping device 10 wipes a predetermined area of a manufacturing facility (not shown) by sandwiching both ends of the hollow wiping device 10 from the left and right and by the urging force of a spring. It is convenient to use a handle 16 that can be rotatably gripped. When such a handle 16 is used, it is easy to directly set the wiping device 10 on the support portion 12 of the sample boat 4 after the wiping operation.

[0019]

Since the present invention is configured as described above, it is not necessary to perform pre-analytical treatments such as extraction and quantitative fractionation of a target component, which makes it easy to evaluate the adhered residue and reduces the time required for one hour. The time required above can be achieved in 5 to 10 minutes.
In addition, since the total amount of the adhered residue that has been wiped is analyzed by carbon, and the total amount of the organic matter is used for evaluating the adhered residue, even if there is contamination by a component other than the conventional target component, it is possible to cope with the problem. Of the adhered residue having a high degree of adhesion. In addition, by devising the handle of the wiping device, it can be prevented from directly touching the analyst's hand, which is useful for preventing contamination from the outside.

Further, since the wiping device is subjected to the measurement and the washing is performed at the same time, the device can be used again for wiping the next adhered residue after the measurement, which is efficient in terms of time and economy.

[Brief description of the drawings]

FIG. 1 is a diagram showing a configuration of a main part of an apparatus for performing a method of the present invention.

FIG. 2 is a diagram showing an example of a wiping device used to carry out the method of the present invention.

FIG. 3 is a view showing an example of a handle of a wiping device used to carry out the method of the present invention.

FIG. 4 is a view showing an example of a support portion of a sample boat of the apparatus for performing the method of the present invention.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... Boat moving rod 4 ... Sample boat 6 ... Combustion tube 7 ... Heating furnace 10 ... Wiping device 12 ... Wiping device support part 13 ... Non-dispersive infrared gas analyzer 16 ... Handle

Claims (2)

(57) [Claims] 1. A wiping device in which fibers made of an inorganic material not containing carbon are fixed to a holder made of an inorganic material containing no carbon, the adhered residue is collected, and the wiping device is taken together with a carrier gas containing oxygen. The carbon residue in the residue is converted to carbon dioxide by combustion and oxidation, and the carbon content is measured to determine the amount of carbon in the residue, thereby evaluating the residue. Object evaluation method. 2. A sample boat on which a sample is placed is introduced into a heating furnace, and the sample is burned and oxidized in a carrier gas containing oxygen to convert carbon in the sample into carbon dioxide. In a device for guiding and measuring to a gas analyzer, a sample boat is provided with a support for detachably supporting a wiping device in which a carbon-free inorganic fiber is fixed to a holder made of a carbon-free inorganic material. Claim 1
For carrying out a method for evaluating the adhesion residue of pulp.