Method development for impurity analysis using the ACQUITY UPLC H-Class System with ACQUITY QDa Detector

Margaret Maziarz

purpose
Proof of ziprasidone hydrochloride and related compounds can be confirmed by qualitative mass spectrometry data obtained using the ACQUITY UPLC ® H-Class System with ACQUITY ® QDaTM Mass Detector during method development.

background
Method development typically involves screening of chromatographic parameters such as columns, organic solvents, buffers, gradient curves, flow rates, and temperatures. Any of these parameters can be optimized to improve resolution to achieve the required analytical quality control requirements.
Subtle changes in pH generally change the relative retention time (elution position) of the compound during reverse phase separation. When studying these separation variables, you must track the change in chromatographic behavior of each component in the sample. At the same time, it is also necessary to identify co-eluting materials.
Failure to track peaks completely and accurately will increase method development time and may not identify significant impurities. In addition, the misidentification or identification of impurities may affect the safety and efficacy of the final drug product. The use of a mass spectrometer allows the analytical laboratory to properly monitor peak retention by mass spectrometry.
The ACQUITY QDa Detector minimizes the need for standard operation and facilitates the development of efficient and durable screening methods to confirm peaks based on retention time.
In this study, we tracked ziprasidone hydrochloride and its USP-specified compounds using qualitative mass spectrometry data obtained with the ACQUITY QDa detector using a range of mobile phases with different pH values. The pH is controlled using the ACQUITY UPLC ® H-Class system combined with Auto•Blend PlusTM technology and contributes to method development.
solution
Use the Auto•Blend Plus technology built into the ACQUITY UPLC H-Class System to set the blend ratio of acidic/alkaline stock buffer to organic/aqueous solvent to achieve a mobile phase with a constant pH. Confirmation of ziprasidone hydrochloride and related compounds using the ACQUITY QDa Detector. In this pH screening study, different ratios of 125 mM formic acid, ammonium hydroxide stock solution, acetonitrile and water were set and mixed by a quaternary pump to obtain mobile phases with pH values ​​of 3.1, 4.0 and 5.0, respectively. Table 1 shows the Auto•Blend Plus method with a pH setting of 3.1. Figure 1 shows the effect of pH on the separation of ziprasidone hydrochloride and related compounds.

As shown in Figure 1, an increase in pH results in an extension of retention of all peaks. Less peaks were observed at a pH of 4.0 compared to pH 3.1 or 5.0. The ACQUITY QDa detector was used to track and identify peaks during method development at different pH values.
Figure 2 shows the use of mass spectrometry to track elution peaks. The peaks were confirmed by mass spectrometry and the tracking of the peak 2 elution sequence was refined in conjunction with UV data.

In summary, the ACQUITY QDa Detector is the perfect complement to the chromatography system, providing mass spectrometry molecular information to analytical scientists without the need for high-end mass spectrometers. Minimize the need for standard testing and simplify the method development process and increase the durability of the method by retaining time to confirm the peak. When used with Empower ® 3 software that can process both optical and mass spectral data, the mass spectral data can be queried through the same workflow as the ACQUITY UPLC PDA Detector data.
to sum up
The ACQUITY QDa detector was used to track sample components during the development of the UPLC ® method for the separation of ziprasidone hydrochloride and its USP specified impurities. The ACQUITY QDa Detector complements optical data with higher quality qualitative mass spectrometry data to confirm components using orthogonal detection techniques.

Overall, the ACQUITY UPLC H-Class System and Auto•Blend Plus technology with the ACQUITY QDa Detector enable complete and fast chromatographic separation and compound identification, greatly simplifying the workflow for laboratory drug analysis.

To download a clear and complete application note, please click: http://?cid=511436&lid=134766907&xcid=x5606&ref=

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