Improving the Data Integrity of Spectrometers
Why Data Integrity Is Important?
The following warning letters have been issued by the FDA, demanding swift response regarding analytical instruments that do not support data integrity.
|Warning Letter: 320-18-55 Issue Date: May 23, 2018
You did not have procedures for reviewing audit trails or electronic data for the Fourier-transform infrared spectroscopy or ultraviolet systems.
|Warning Letter: 320-17-25 Issue Date: February 24, 2017
Our investigator observed that your laboratory systems lacked controls to prevent your staff from altering or deleting electronic data. Analysts manipulated and deleted audit trails. You lacked adequate controls for all HPLC, gas chromatography, and ultra-violet systems.
|Warning Letter: 320-17-01 lssue Date: October 13, 2016
In response, to this letter, provide details of your retrospective review of HPLC and other laboratory data, such as Fourier transform infrared spectroscopy, gas chromatography, UV spectrophotometry, and (b)(4) analyzer data.
|Warning Letter: 320-15-09 lssue Date: April 6, 2015
You lacked controls to prevent the unauthorized manipulation of your laboratory's electronic raw data. Specifically, your infrared (IR) spectrometer did not have access controls to prevent deletion or alteration of raw data.
Data Integrity and Report Set
Data integrity refers to the completeness of data, with nothing missing or inconsistent. In other words, not only the data itself but also the metadata (the results of work that require human intervention, such as specifying conditions and analyzing analysis data) must be presented in a visible form, and verified together with the data. This is achieved by the Report Set.
What Is Shimadzu LabSolutions Report Set?
This function gathers operational information (operations and settings that require human intervention) distributed within the software, and collects it in a single report. Much like an electronic book, the content can be checked while turning the pages, which eliminates the need to check operations and settings by switching between windows and tab pages.
Procedures for Creating a Report Set*1,*2 with a Shimadzu Spectrometer
The procedures for creating a Report Set with a spectrometer follow the sequence for chromatographs, so the procedures are just as simple as with a chromatograph.
*1: As of January 2019, the following functions (1) to (2) are not yet supported for UV, FTIR, and RF Report Sets.
(1) ID assignment to measurement methods
(2) Avoidance of duplicate printing of measurement methods for multiple data sets
*2: UV, FTIR, and RF Report Sets are supported by the LabSolutions CS network and LabSolutions DB standalone.
*3: In terms of file selection when creating report sets, for UV photometric data, if a single file is selected, a Report Set including any related files will be created. In contrast, with UV, FTIR, and RF spectral measurements, if multiple files are related, manually select those files.
*4: In sequential measurement, the report can be created from dataset batch. (A series of data report can be created)
*5: A log is recorded during measurements. If a postrun analysis is performed, a log will also be recorded during the postrun analysis.
*6: Locked files can only be unlocked by users with the relevant rights.
Analysis Sequence (Optional)
Ensuring data integrity requires a system that shows no data manipulation has occurred. Shimadzu has achieved this through the introduction of its Analysis Sequence for spectrometers. Using the Analysis Sequence, it is possible to verify that the full chain of analysis has been carried out according to experimental protocol (or SOP). The LabSolutions Analysis Sequence (optional) provides a three-step workflow:
- A sequence is put together according to a given experimental protocol (or SOP). See the flow below for reference.
- The operator conducts analysis in the order shown by the sequence file.
- After analysis, a report set is created from the sequence file used in the analysis. The experiment leader uses the report set to review the data chain generated by the sequence.
Until now, a problematic issue with data integrity in spectrometers has been the existence of orphan data (data which is isolated and not reviewed, despite being used in the analysis). However, the LabSolutions Analysis Sequence option not only meets the requirements for data integrity by preventing the creation of orphan data, but also allows for highly efficient spectrometer operation.
Note 1) This is not compatible with LabSolutions RF, which controls the RF-6000 spectrofluorophotometer. Compatibility is expected shortly.
Note 2) This is only compatible with LabSolutions UV-Vis, the software that controls UV-Vis spectrophotometers. It is not compatible with UVProbe. Future compatibility with UVProbe is not expected. If compatibility is required, purchase LabSolutions UV-Vis, and then purchase Analysis Sequence separately.
Compatibility with Data Integrity for IR Microscopes (Optional)
The main application of IR microscopes is contaminant analysis, and compatibility with standards is not required. However, such instruments are often installed in the same laboratory as instruments used for confirmatory test applications. During inspections, it is necessary to explain the lack of compatibility with standards to inspectors. To avoid this troublesome process, the control software for IR microscopes for contaminant analysis applications is now compatible with data integrity. The operations are simple. Run LabSolutions IR, the Shimadzu software used for confirmatory test applications. Click [AIM] for IR microscope measurements, which is built into the software. This will display the existing AIMsolution program. Then configure the various conditions, and start the measurements. After the measurements are finished, the data obtained is automatically transferred to the LabSolutions IR software, after which it is transferred up the line.
Note 1) Data integrity compatibility is not available when using the AIMsolution mapping software.
Note 2) The measurements are performed with AIMsolution. This is not compatible with Analysis Sequence.