Determination of 10 residual solvents in ceftriaxone sodium and quality evaluation by direct injection gas chromatography-tandem mass spectrometry
Objective To establish a direct injection gas chromatography-tandem mass spectrometry(GC-MS/MS)method to determine 10 residual solvents in ceftriaxone sodium and evaluate its quality.Methods An Agilent J&W DB-624UI capillary column(60 m× 0.250 mm,1.4 μm)was used.The temperature of injection was 235 ℃,the initial column temperature was 30 ℃,held for 12 min and then increased at a rate of 5 ℃·min-1 to 100 ℃,held for 1 min,and finally increased at a rate of 50 ℃·min-1 to 235 ℃,held for 10 min.The flow rate was 3 mL·min-1.Splitless injection was adopted,and the injection volume was 0.2 μL.The mass spectrometer was operated with the mass scanning combining selective ion monitoring,n-butanol was used for direct-injection detection,and external standard method was used for quantification.Plackett-Burman design combined with Pareto chart was used to determine the factors influencing the robustness of the method.The method was used to measure residual solvents in 51 batches from 51 producers.Results The 10 residual solvents had good linear relationship within their respective concentration ranges(r＞0.999);the recoveries ranged 99.7％～103.9％,with RSD less than 2％;the detection limits ranged 0.006～67.750 μg·g-1 Acetone was detected in 51 batches of samples while methanol,acetonitrile and isopropanol were partially detected.Conclusion The method is simple,accurate and reliable,with few samples needed,and easy availability of reagents.It can be used for the determination and quality evaluation of residual solvents in ceftriaxone sodium.
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