Determination of the trace of carbon disulfide in melocillin sodium for injection by headspace-gas chromatography
Objective This study established a method for the determination of CS2 in mezlocillin sodium for injection by headspace-gas chromatography.Methods The method was used with the capillary column DB-624(30 m× 0.53 mm×3 μm)andthe temperature of the injection port was 160 ℃.The column temperature was programmed(the initial column temperature was 40 ℃ and kept for 5 min at a speed of 60 ℃/min,until raised to 160 ℃ and kept for 8 min).The sample was detected by a flame photometric detector(FPD)with a heater and auxiliary transmission line temperature of 200 ℃ and a combustion chamber temperature of 125 ℃.The equilibrium temperature of the headspace bottle was 80 ℃ and the balance time was 30 min.Results The mass concentration of CS2 had a quadratic relationship with the peak area in the concentration range of 0.04～0.8 μg/mL,and the detection limit(LOD)was 0.01 μg/mL.CS2 was detected in 87 batches of 157 samples from 12 manufacturing enterprises,and 33 batches of samples exceeded the proposed limit(3.2 μg/g).The CS2 in the samples was mainly migrated from the rubber plug.Conclusion The method had good reproducibility,high accuracy and could be used for the detection of trace amounts of CS2 in this product,which provided a quality basis for the selection of suitable stoppers for injection drug manufacturers.
Mezlocillin sodium for injectionCarbon disulfide(CS2)Headspace-gas chromatographyRubber closuresQuality control
万方数据
维普
