CN-122029422-A - Method for producing sample for analysis and verification of fluorescent X-ray analysis device, and method for analysis and verification of fluorescent X-ray analysis device

Abstract

The target elements including Cd, pb, as, hg, co, V and Ni are divided into a plurality of groups so that As and Pb are the same group and the As and Pb and Hg are different groups, and for each group, a liquid (12, 121-128) containing the target element belonging to the group is added to a powder (11) composed of a material not containing any of the target elements, and mixed so that the target elements belonging to the group are each of a predetermined concentration.

Inventors

• NAKAO TAKAMI

Assignees

• 株式会社岛津制作所

Dates

Publication Date

20260512

Application Date

20240628

Priority Date

20231030

Claims (10)

1. 1. A method for producing a sample for analysis and verification of a fluorescent X-ray analyzer, characterized in that target elements including Cd, pb, as, hg, co, V and Ni are divided into a plurality of groups such that As and Pb are the same group and the As and Pb and Hg are different groups, and for each of the plurality of groups, a liquid containing the target element belonging to the group is added to a powder composed of a material not containing any of the target elements and mixed so that the target elements belonging to the group are each of a predetermined concentration.
2. 2. The method for producing a sample for analysis and verification by a fluorescent X-ray analysis apparatus according to claim 1, wherein Hg and Ni and/or Hg and Co are different from each other.
3. 3. The method for producing a sample for analysis and verification by a fluorescent X-ray analysis apparatus according to claim 1, wherein Hg and V belong to the same group.
4. 4. The method for producing a sample for analysis and verification of a fluorescent X-ray analysis apparatus according to claim 1, wherein the target element further comprises Pd.
5. 5. The method for producing a sample for analytical verification by a fluorescent X-ray analysis apparatus according to claim 4, wherein Hg and Pd belong to the same group.
6. 6. The method for producing a sample for analysis and verification by a fluorescent X-ray analysis apparatus according to claim 1, wherein the plurality of groups are composed of a1 st group composed of Cd, pb, as, co and Ni and a2 nd group composed of Hg and V.
7. 7. The method for producing a sample for analysis and verification by a fluorescent X-ray analysis apparatus as claimed in claim 6, wherein the target element further contains Pd belonging to the group 2.
8. 8. The method for producing a sample for analysis and verification by a fluorescent X-ray analysis apparatus according to claim 1, wherein one of the plurality of groups contains Hg only in the target element.
9. 9. The method for producing a sample for analysis and verification by a fluorescent X-ray analysis apparatus according to claim 1, wherein a plurality of liquids each containing 1 kind of target element belonging to each of the plurality of groups are added to different positions of the powder, and the powder is stirred after the plurality of liquids are dried.
10. 10. An analysis and verification method of a fluorescent X-ray analysis apparatus, characterized in that, for a plurality of analysis and verification samples produced by the production method of an analysis and verification sample of a fluorescent X-ray analysis apparatus according to any one of claims 1 to 9, fluorescent X-ray analysis is performed by using a fluorescent X-ray analysis apparatus as an analysis and verification object, respectively, to measure the concentration of the object element, and it is determined whether or not the difference between the obtained concentration and the predetermined concentration is within a predetermined range.

Description

Method for producing sample for analysis and verification of fluorescent X-ray analysis device, and method for analysis and verification of fluorescent X-ray analysis device Technical Field The present invention relates to a method for producing a sample used for performing analysis verification (validation test) of a fluorescent X-ray analysis apparatus, and an analysis verification method of a fluorescent X-ray analysis apparatus using the sample. Background If a harmful metal element is mixed as an impurity into a pharmaceutical product, food or the like, there is a possibility that health hazard is given to a person who ingests the pharmaceutical product, food or the like. Therefore, a standard for regulating the concentration of a specific metal element is established. In particular, in the field of pharmaceuticals, international medical and regulatory conference （ICH：International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use） sets an international standard called "elemental impurity guideline Q3D" (Guideline for Elemental Impurities Q3D, hereinafter referred to as "ICH Q3D") (see non-patent document 1). In ICH Q3D, a daily allowable intake amount was defined for 24 metal elements, and the allowable concentration of each preparation was found from the daily allowable intake amount. The 24 kinds of metal elements are classified into 4 kinds (type 1, type 2A, type 2B, and type 3) according to their toxicity intensity and the possibility of mixing into the pharmaceutical products. Category 1 consists of 4 elements, cd (cadmium), pb (lead), as (arsenic) and Hg (mercury), of which the toxicity is particularly strong among the 24 elements. Category 2A is composed of 3 elements, i.e., co (cobalt), V (vanadium), and Ni (nickel), which are derived from natural substances and have a high possibility of being mixed into pharmaceuticals. The category 2B is composed of 10 elements such as Pd (palladium) which may be mixed into the medicine from a substance used in the production process of the catalyst or the like, although the possibility of mixing from natural substances is low. Category 3 consists of 7 elements which are less toxic than the 17 elements described above, do not require evaluation (evaluation) in oral formulations, but belong to the evaluation subjects in injections or inhalants. When the concentration of the metal element in the pharmaceutical is evaluated based on ICH Q3D, the evaluation target contains at least 7 elements belonging to the categories 1 and 2A. Among the 10 elements belonging to class 2B, if there is an element that may be mixed in at the time of manufacturing the pharmaceutical, the element is also included in the evaluation object. For example, in evaluating an oral preparation manufactured using Pd, 8 elements obtained by adding Pd to the 7 elements are used as evaluation targets. Pd is an element used as a catalyst in the production of many medicines. In the case of an injection or an inhalant, a part or all of 7 elements belonging to the category 3 are included in the evaluation target as needed. In non-patent document 1, inductively coupled plasma mass spectrometry (ICP-MS) is used as a concentration analysis method of an element to be evaluated, but ICP-MS has a problem that sample pretreatment is time-consuming and laborious. In contrast, a fluorescent X-ray analysis method that facilitates sample pretreatment is proposed to analyze the concentration of an element to be evaluated (non-patent document 2). In the fluorescent X-ray analysis method, the pretreatment of the sample is only required to pulverize the medicinal product into a uniform powder. In the fluorescent X-ray analysis method, in order to confirm that the device and analysis conditions for analyzing the concentration of the element to be evaluated are appropriate, it is necessary to periodically perform analysis verification, that is, to perform fluorescent X-ray analysis on a sample for analysis verification containing the element to be evaluated at a known concentration, to confirm whether or not the correct concentration has been obtained. Since the original analyte is measured in a powder state, the sample for analysis and verification is prepared by adding a predetermined amount of standard solution containing a predetermined concentration of the target element to a powder (for example, cellulose powder as a pharmaceutical additive) and mixing the mixture. Prior art literature Patent literature Non-patent document 1,2, roxie, et al, "pharmaceutical element impurity guide (ICH Q3D) and ICP-MS: status seen from the standpoint of analysis responsible person", kanto Chemicals, THE CHEMICAL TIMES, tongju No. 255, pages 7-13, release 1 in 2020 Non-patent document 2, "management of elemental impurities in pharmaceuticals", [ on-line ], shimadzu corporation, [2023, 10, 30, suo, internet <https://www.an.shimadzu.co.jp/products/elemental-analysis/edx-fs/pharmaceutical-eleme