Detection of Residual Solvents in Daptomycin by Headspace Gas Chromatography
Objective To establish a headspace gas chromatography method for the determination of three organic solvent residues in daptomycin.Methods The chromatographic column was the Agilent DB-624 capillary column(60 m×0.53 mm,3.0 μm),the carrier gas was nitrogen with a flow rate of 5.0 mL/min,the temperature was programmed,the flame ionization detector(FID)was adopted,the inlet temperature was 200℃,the detector temperature was 230℃,the split ratio was 5∶1(V/V),the balance temperature of headspace bottle was 85℃,the balance time was 30 min,and injection volume was 1 μL.Results The linear ranges of ethanol,isopropanol and n-butanol were 10-200 μg/mL(r=1.000 0).The limits of detection(LOD)of the above three components were 0.75,0.30,0.75 μg/mL,and their limits of quantification(LOQ)were 2.50,1.01,2.50 μg/mL,respectively.The RSDs of precision,stability,and repeatability tests were all lower than 2.0%.The average recovery rates of the above three components were 101.85%,101.65%,102.33%,with the RSDs of 0.59%,0.77%,0.78%respectively(n=9).Conclusion This method is specific,sensitive and precise,which can be used for the determination of the above three organic solvent residues in daptomycin.The residual amount of organic solvents detected in three batches of samples is far below the limit of national standard.
daptomycinfreeze-drying processorganic solvent residuesolubilityredissolution time
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