Determination of 1,3-dichloro-2-propyl alcohol residues in Ornidazole by GC-MS
OBJECTIVE To detect the 1,3-dichloro-2-propanol(1,3-DCP)in Ornidazole by GC-MS.METHODS The capillary column with 100％polyethylene glycol(PEG-20M)as fixed liquid was used for separation.Mass spectrometry adopted electron bombardment ionization source(EI)ionization,ion source temperature of 230 ℃,ionization energy of 70 eV,quadrupole temperature of 150 ℃,mass scanning range of 40-450 amu,1,3-DCP quantitative ion of m/z 79,and qualitative ion of m/z 81.RESULTS The linear relationship of 1,3-DCP was good in the concentration range of 1.0-5.0 mg·L-1,and the limit of detection and limit of quantitation were 0.2489 and 0.7716 mg·L-1,respectively.The recoveries were 92.48％-98.39％with RSDs less than 5.0％.The method was used to determine 1,3-DCP in 27 batches of ornidazole raw materials,among which 10 batches of Ornidazole raw materials contained 1,3-DCP exceeded the limit value,and the rest met the requirements.CONCLUSION The method is simple,accurate,sensitive and reproducible,which can be used for the determination of 1,3-DCP residue in ornidazole.
OrnidazoleAPI1,3-dichloro-2-propanolThe amount of residueGas chromatography-mass spectrometry
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