Analysis of genotoxic impurity chloropropanol in hydroxypropyl distarch phosphate by GC-MS
Objective:To establish a method for the detection of genetic impurity chloropropanol in hydroxypropyl distarch phosphate(HPDSP).Methods:The method was performed with Agilent VF-WAX capillary column and temperature programmed by GC-MS.The initial temperature was 80 ℃ for 8 min,then increased to 220 ℃ at the rate of 35 ℃·min-1 and maintained for 5 min with the flow rate of 2 mL·min-1.The temperature of inlet was 200 ℃,and the injection volume was 1 μL without split.The detector was electron impact(EI)with selected ion monitoring(SIM)mode and ion source temperature at 230 ℃.The m/z of qualitative ions of 1-chloro-2-pro-panol were 45,43,79,81,and the m/z of quantitative ion was 79.The m/z of qualitative ions of 2-chloro-1-propanol were m/z 58,62,63,64,65,and m/z of the quantitative ion was 62.Results:Good linear was achieved in the range of 20.04 ng·mL-1 to 1 002 ng·mL-1(r=0.999 8,n=7)and the recovery rate ranged from 93.7％to 117.1％for 1-chloro-2-propanol.The contents of chloropropanol in 9 batches were within the range of 0.000 006％-0.000 08％.Conclusion:The method shows the advantages of high sensitivity,good accuracy,linearity and can be used for the detection of genetic impurities in HPDSP.
hydroxypropyl distarch phosphate(HPDSP)detection of genetic impurityGC-MS1-chloro-2-propanol2-chloro-1-propanolchloropropanol
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