Participants in ShootOut-2002

Fred McClure, Coordinator of ShootOut-2002 Session

Designing the Best Possible Calibration Transfer Procedure

Objectives of the Shootout:

Spectra of 654 pharmaceutical tablets [1] from two Multitab spectrometers [2]  (FossNIRsystems, Silverspring, MD) will be the basis of the ShootOut at the next Chambersburg meeting (August 10-16, 2002). All tablets were measured in the transmittance mode.  Each individual tablet was subsequently analyzed for ASSAY value, tablet weight, and tablet hardness. All log (1/T) spectra cover the region from 600 to 1898 nm in 2 nm increments.  Spectra were collected with Foss-NIRSystems "Vision" software, but have been exported to NSAS *.DA format, to JCAMP-DX and to CSAS format.  Other formats may be available per participant request.  Data from each instrument has been split into a calibration file (155 spectra), and a validation file (459 spectra). In addition, a small test file (40 spectra) from each instrument is available for testing calibrations.

The challenge is to develop the best possible calibration for the ASSAY value on one instrument, and to provide the best means of transferring the calibration to the other instrument. The reference method has an error of +/- 1.3 mg on these tablets with a nominal value of 200 mg per tablet. The data set includes tablets with a wide ASSAY range, 152 to 239 mg, for developing calibration(s). No deliberate outliers are included in the data set, but there may be outliers due to experimental errors.  The name of the active ingredient in these tablets can not be disclosed for proprietary reasons.

Data Files: There are 24 separate files in NSAS (*.da and .cn) and J-CAMP (*.dx) and CSAS formats.  The file list below details the filenames, approximate file size, number spectra (constituents) in each file and file format. Spectra from Inst#1 and Inst#2 appear in the same order in the respective files.  The following notations are used for sample IDs:

 

[1] Gary E. Ritchie, Chairman NIRVWoG and Sr. Scientist, Pharmaceutical Analysis/New Technology, Purdue Pharma L.P., 444 Saw Mill River Road, Ardsley, NY 10502

[2] http://www.foss.dk/c/p/solutions/products/showprodfamily.asp?prodfamilypkid=98

 

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DATA FILES for ShootOut-2002

August 10-16, 2002

Wilson College, Chambersburg, PA

   

   
Filename

File Size (KB)

Number

Format

Calibra1

410

155

CSAS

Calibra1.cn

20

155

NSAS (const)

Calibra1.da

427

155

NSAS (spec)

Calibra1.dx

1,586

155

J-Camp

Calibra2

410

155

CSAS

Calibra2.cn

20

155

NSAS (const)

Calibra2.da

427

155

NSAS (spec)

Calibra2.dx

1,587

155

J-Camp

Test1

1,214

460

CSAS

Test1.cn

58

460

NSAS (const)

Test1.da

1,265

460

NSAS (spec)

Test1.dx

4,707

460

J-Camp

Test2

1,214

460

CSAS

Test2.cn

58

460

NSAS (const)

Test2.da

1,265

460

NSAS (spec)

Test2.dx

4,709

460

J-Camp

Validat1

106

40

CSAS

Validat1.cn

6

40

NSAS (const)

Validat1.da

110

40

NSAS (spec)

Validat1.dx

346

40

J-Camp

Validat2

106

40

CSAS

Validat2.cn

6

40

NSAS (const)

Validat2.da

110

40

NSAS (spec)

Validat2.dx

346

40

J-Camp