LC-MS/MS determination of Synercid injections

Area of Science:

• Analytical Chemistry
• Pharmaceutical Analysis
• Mass Spectrometry

Background:

• Synercid, a combination of quinupristin and dalfopristin, requires precise quantification for therapeutic efficacy.
• Accurate determination of antibiotic content is crucial for quality control and stability monitoring.

Purpose of the Study:

• To develop and validate a rapid, specific, and sensitive High-Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS/MS) method.
• To quantify quinupristin and dalfopristin in Synercid injections.
• To assess the method's suitability for tracking drug stability and compatibility.

Main Methods:

• Utilized positive electrospray tandem mass spectrometry (+ESI-MS/MS).
• Employed multiple reaction monitoring (MRM) transitions for quinupristin (1023.05>134.34) and dalfopristin (691.87>166.26).
• Performed quantitation using peak area measurements with weighed linear regression and validated linearity up to 4000 ng/mL (quinupristin) and 1920 ng/mL (dalfopristin).

Main Results:

• Achieved a rapid assay cycle time of approximately 2.0 minutes.
• Established low limits of quantitation: 1000 ng/mL for quinupristin and 480 ng/mL for dalfopristin.
• Demonstrated high precision (%RSD: 1.3-4.2%) and accuracy (%DEV: -7.5 to +9.1%), with excellent recoveries (97.8-103.8%).
• Confirmed the 30:70 (w/w) ratio of quinupristin to dalfopristin in Synercid injections through slope analysis of calibration curves.

Conclusions:

• The developed HPLC-MS/MS method is rapid, specific, and accurate for quantifying quinupristin and dalfopristin in Synercid injections.
• This validated method is suitable for routine quality control, including content determination, stability studies, and compatibility assessments.
• The method's efficiency and reliability support pharmaceutical analysis and ensure the quality of Synercid formulations.