Sample preparation device to form a matrix film for matrix assisted laser desorption/ionization method

• US 9,334,569 B2
• Filed: 11/12/2012
• Issued: 05/10/2016
• Est. Priority Date: 12/02/2011
• Status: Active Grant

• Current Assignee: Shimadzu Corporation
• Original Assignee: Shimadzu Corporation
• Inventors: Takahashi, Kazuteru, Ogawa, Kiyoshi
• Primary Examiner(s): Thomas, Binu
• Application Number:
  US13/674,745
• Publication Number:
  US 20130171349A1
• Time in Patent Office: 1,275 Days
• Field of Search: None
• US Class Current: 1/1
• CPC Class Codes: C23C 14/12 Organic material
• CPC Class Codes: C23C 14/24 Vacuum evaporation
• CPC Class Codes: C23C 14/54 Controlling or regulating the coating process
• CPC Class Codes: C23C 14/547 using optical methods
• CPC Class Codes: C23C 14/548 Controlling the composition
• CPC Class Codes: C23C 16/52 Controlling or regulating the coating process C23C16/45557, C23C16/279 take precedence
• CPC Class Codes: G01B 11/0625 with measurement of absorption or reflection

Abstract

To provide a sample preparation device that is appropriate for the formation of a matrix film for MALDI through vacuum vapor deposition. A sample preparation device is provided with: a sample substrate support unit 23 for supporting a substance to be analyzed on a substrate S so that the substance faces a vapor deposition source 21 for a matrix substance J; a light amount measurement unit for irradiating a matrix film vapor deposited on the substrate S with measurement light diagonally and detecting the amount of measurement light that has transmitted through or has been reflected from the above-described matrix film diagonally; and an adhesion prevention means 23a for preventing the matrix substance that has flown off from the above-described vapor deposition source 21 from adhering to the above-described light amount measurement unit.

Claims

1. A sample preparation apparatus for forming a matrix film at least on a subject pasted on a sample substrate to prepare a sample, the subject in the sample being analyzed using a matrix assisted laser desorption/ionization method, the sample preparation apparatus comprising:

a vacuum container;

a vapor deposition source disposed in the vacuum container and configured to heat a matrix material so that the matrix material is vapor deposited on the subject to form the matrix film;

a sample substrate support configured to support the sample substrate so that the subject to be analyzed on the sample substrate faces the vapor deposition source;

a light source disposed in the vacuum container to emit light obliquely incident on the matrix film on said sample substrate, the light source having a light emitting surface from which the light is emitted, and

a light detector disposed in the vacuum chamber to receive light from the matrix film for detecting an amount of light transmitted through or reflected from the matrix film, the light detector having a light receiving surface through which the light from the matrix film is received;

an adhesion protector configured to prevent the matrix material from adhering to the light source and the light detector during the vapor deposition of the matrix material on the subject; and

a processor, associated with the light source and the light detector, configured to control the vapor deposition source to form the matrix film in an area of the sample to have a predefined thickness for the matrix assisted laser desorption/ionization method, wherein

the adhesion protector includes;

a first aperture member disposed in front of the light emitting surface of the light source, the first aperture member having an aperture through which the light from the light source passes, the aperture of the first aperture member being positioned to arrange an optical axis of the light from the light source to be inclined with respect to a path of the matrix material from the vapor deposition source to the sample substrate for vapor deposition; and

a second aperture member disposed in front of the light receiving surface of the light detector, the second aperture member having an aperture through which the light from the matrix film passes, the aperture of the second aperture member being positioned to arrange an optical axis of the light from the matrix film to be inclined with respect to the path of the matrix material from the vapor deposition source to the sample substrate for vapor deposition.

2. The sample preparation device according to claim 1, wherein

said sample substrate support is formed of a support plate where an opening through which the subject to be analyzed on said sample substrate faces said vapor deposition source is provided,

said support plate is formed so as to work as an adhesion prevention plate in such a manner that the matrix material from said vapor deposition source is prevented from coming around to a space on a side opposite to said vapor deposition source with the support plate in between when said sample substrate is placed on said opening, and

said support plate works as the adhesion protector for said light source or said light detector in a case where the light source or the light detector is provided in said space on the opposite side.

3. The sample preparation device according to claim 1, wherein the adhesion protector includes an adhesion prevention plate made of a cover for covering an outside of the light source or said light detector, except for the light emitting surface through which light is emitted from the light source or the light receiving surface through which light enters into the light detector.

4. The sample preparation device according to claim 1, wherein one of said light source and said light detector is provided on the vapor deposition source side of said sample substrate support, and the other is provided on a side opposite to the vapor deposition source with said sample substrate support in between so that the amount of light that has transmitted through said matrix film is detected.

5. The sample preparation device according to claim 1, further comprising a storage for storing film thickness reference information for finding a film thickness from the amount of light to be transmitted through or reflected from the matrix film by measuring the relationship between the film thickness of the matrix film on said sample substrate and the amount of light to be transmitted through or reflected from the matrix film, wherein

the processor is further configured to control the film thickness of the matrix film to be formed on the sample substrate by allowing the light source and detector to measure the amount of light from the matrix film being vapor deposited on the sample substrate and by controlling a degree of heating of said vapor deposition source on the basis of the measured amount of light and said film thickness reference information.

7. The sample preparation device according to claim 1, wherein the adhesion protector further includes:

a third aperture member disposed in front of the first aperture member, the light emitting surface, the first aperture member, and the third aperture member being arranged in that order along the optical axis of the light from the light source, the third aperture member having an aperture through which the light from the light source passes, the apertures of the first and third aperture members being positioned to arrange the optical axis of the light from the light source to be inclined with respect to the path of the matrix material from the vapor deposition source to the sample substrate for vapor deposition, and

a fourth aperture member disposed in front of the second aperture member, the light receiving surface, the second aperture member, and the fourth aperture member being arranged in that order along the optical axis of the light from the matrix film, the fourth aperture member having an aperture through which the light from the matrix film passes, the apertures of the second and fourth aperture members being positioned to arrange the optical axis of the light from the matrix film to be inclined with respect to the path of the matrix material from the vapor deposition source to the sample substrate for vapor deposition.

6. A sample preparation device for preparing a sample to be analyzed using a matrix assisted laser desorption/ionization method by forming through vacuum vapor deposition, at least on a substance to be analyzed on a sample substrate to which the substance to be analyzed is pasted, a matrix film where two types of matrix substances A and B are mixed, comprising:

two vapor deposition sources for independently heating said two types of matrix substances A and B within a vacuum container so that the matrix substances A and B are vapor deposited;

a sample substrate support unit for supporting the sample substrate so that the matrix substances A and B to be analyzed on said sample substrate faces both of said two vapor deposition sources;

a light amount measurement unit made up of a light source, which is provided within said vacuum container and diagonally irradiates the matrix film vapor deposited on said sample substrate with light for measurement, and a light detector for detecting an amount of light for measurement that has diagonally transmitted from the matrix film vapor deposited on said sample substrate, the light source having a light emitting surface from which the light is emitted, the light detector having a light receiving surface through which the light from the matrix film is received; and

an adhesion protector configured to prevent the matrix substances A and B from adhering to the light source and the light detector during the vapor deposition of the matrix substances A and B, wherein

said light amount measurement unit has the light source using light with a certain wavelength that transmits through the matrix substance A, and at the same time is absorbed by the matrix substance B, and

the adhesion protector includes;

a first aperture member disposed in front of the light emitting surface of the light source, the first aperture member having an aperture through which the light from the light source passes, the aperture of the first aperture member being positioned to arrange an optical axis of the light from the light source to be inclined with respect to a path of the matrix substances A and B from the two vapor deposition sources to the sample substrate for vapor deposition; and

a second aperture member disposed in front of the light receiving surface of the light detector, the second aperture member having an aperture through which the light from the matrix film passes, the aperture of the second aperture member being positioned to arrange an optical axis of the light from the matrix film to be inclined with respect to the path of the matrix substances A and B from the two vapor deposition sources to the sample substrate for vapor deposition.