Optimization

 

Reduce the Number of Data Points Using Experimental Design

Box-Behnken design and central composite design can shorten analysis times because they require fewer data points than full factorial design. For example, if determining the three optimal levels for the organic mobile phase mixture ratio, pump gradient conditions, and column oven temperature, full factorial design requires 27 data points (3 × 3 × 3) for optimization whereas Box-Behnken design requires 13 points and central composite design requires 15 points.

Comparison of Data Points Required for Each Experimental Design Method

 

 

Easily Create an Analysis Schedule Experimental Design

The process of creating the vast number of method files and analysis schedules required for screening can be completed quickly by simply following steps (1) to (6) below. The mobile phase and column to be used can be selected with a single click and a comprehensive schedule reflecting column equilibration and blank analysis is generated automatically. That not only improves operational efficiency, but also can reduce human errors. The experimental design to be used can also be selected with a single click.

Experimental Design Selection Window

Easy Creation of Analysis Schedule

Quickly Find Optimal Condition

Because screening generates as many chromatograms as the number of conditions considered, they must be evaluated to determine which is optimal. If all the chromatograms had to be scrutinized by a human, it would be very tedious. LabSolutions MD can quickly and easily find optimal analytical conditions using equation (1) below to quantitatively evaluate the separation status resulting from each analytical condition. 

*Method Scouting Solution can be used in conjunction with optional software multi-data reporting.

E = P×(Rs1+Rs2+…RsP) … (Eq. 1)

The evaluation value (E) is calculated as the number of peaks detected (P) multiplied by the sum of the separation level (Rs) for all peaks.

Comparison of Chromatograms

 

 

Identify the Most Robust Analytical Condition by Design Space

Analytical Intelligence

Visualize the Factor-Response Relationship, and Specify the Most Robust Analytical Conditions

After the pH level of aqueous mobile phase and column are selected in the screening phase, analytical condition is further optimized by considering the parameters of mixture ratio of organic mobile phase (30, 40, 50, 60, 70 %), oven temperature (35, 40, 45 °C), and final concentration of gradient program (75, 80, 85 %). The effect on separation of these parameters are shown by design space with the mixture ratio of organic mobile phase on the vertical axis and oven temperature on the horizontal axis.

Most Robust Analytical Conditions

Overlaying the design spaces makes it evident that the optimal analytical conditions are as follows: organic solvent mixture ratio of 60 %, column oven temperature of 42 °C, and gradient final concentration of 75 %. It is possible to search not only for the degree of separation and the symmetry factor, but also the optimal analytical conditions considering the analysis time. Robust analytical conditions can be specified without relying on intuition or experience by utilizing design space.

Analytical Intelligence

Simulation of Chromatogram

By clicking any point in design space (e.g. point A : blue square in the black circle), simulated chromatogram can be displayed. This function of chromatogram simulation allows to check how the separation will change through any conditions quickly without running any analysis.

Simulation of Chromatogram

* Mobile Phase B A: Mobile phase A (acetonitrile) from Pump B
The black dots in the figure are points where the analysis was implemented.

Formula

 

Evaluating Robustness Using Iterative Experimental Design

Robustness Evaluation

LabSolutions MD can create sequential experimental design to perform robustness evaluation. Robustness evaluation is important to understand how the variations of parameters will affect results and ensure the reliability of method. LabSolutions MD creates sequential experimental design automatically by changing the parameters of optimized method in a small range to evaluate the robustness. Specifically, mixture ratio of organic mobile phase by 1 % (59, 60, 61 %) and oven temperature by 1 °C (41, 42, 43 °C) (white circles in the right figure) to verify the effect on separation.

 

Below shows chromatograms obtained for robustness evaluation. The effect of variation of the parameters on separation is very small, showing robustness of the optimized method constructed by design space.

Chromatograms of Robustness Evaluation at each Data Point

Chromatograms Obtained at Each Robustness Validation Data Point

Analytical Intelligence

Automatic Identification of Compounds by Peak Tracking (i-PeakTracer™)

Automatic Identification of Compounds by Peak Tracking

Ensure Data Integrity by Database Management

It is easy to check analysis results using LabSolutions MD because all associated information, such as the experimental design, design space, and chromatograms, are output in a report. It also ensures data integrity by managing outputted reports together with the corresponding experimental design file, method file, batch file, and data file within a LabSolutions database.

Due to the seamless integration of all process steps, including creating an experimental design, acquiring data, and all method development steps in the design space, LabSolutions MD eliminates the need for any time-consuming file importing or exporting steps.

Database of LabSolutions

 

Automated Columns and Mobile Phases Switching

Nexera™ Series

These ultra high performance liquid chromatographs have a maximum pressure capacity of 130 MPa and support up to 192 combinations of 8 types of mobile phases and 12 types of columns (4 × 4 × 12).

LCMS System

 

i-Series

 

These space-efficient and cost-efficient integrated LC systems support pressures up to 70 MPa.

i-Series

 

Supercritical Fluid Chromatograph Nexera/UCs UHPLC/SFC Switching System

  • Optimized for method investigation of chiral compounds
  • Also compatible with LC/SFC switching, and can investigate various separation modes
Nexera/UCs UHPLC/SFC

LabSolutions MD doesn’t support SFC system.

 

Automated Mobile Phase Blending

The mobile phase blending functionality can dramatically reduce the amount of time previously required for mobile phase preparation by automatically preparing mobile phases with the user-specified pH level or the organic mobile phase mixture ratio using only a few types of mobile phases prepared in advance. i-Series systems can use a low-pressure gradient to blend up to two types of aqueous and two types of organic mobile phases.

Mobile Phase Blending Functionality Reduces Labor

Automatic Mobile Phase Preparation Using the Mobile Phase Blending Functionality
(in Nexera systems configured with high-pressure gradient capability)

Maximizing Productivity with LCMS-2050

LCMS-2050

 

The LCMS-2050 is a single quadrupole MS that combines revolutionary technology with the ease of use as an LC detector. This system features a wide mass range (m/z 2 to 2,000), a quick start as fast as six minutes, and easy, tool-free maintenance. It can fit into basic LC systems with its space saving design. For details, refer to the catalog “LCMS-2050 Liquid Chromatograph Mass Spectrometer (C146-E442)”.

 

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