Determination of Sulfonate Genotoxic Impurities in Lenvatinib Mesilate Capsules by GC-MS
Objective:To establish a method for the determination of sulfonate genotoxic impurities in Lenvatinib Mesilate Capsules by GC-MS.Methods:Agilent DB-624 capillary column(30 m×0.32 mm×1.8 μm)was used,the initial temperature was 120 ℃,maintained for 5 minutes,and then increased to 230 ℃ at a heating rate of 25 ℃·min-1 for 10 minutes;The sample inlet temperature was set to 250 ℃;The carrier gas was helium,the flow rate was 1.5 mL·min-1 in a constant flow mode;The split ratio was 5∶1,and the injection volume was 1μL;The mass spectrometry detector was an electron bombardment ion source(EI source),voltage was 70 eV,interface temperature was 280 ℃,ion source temperature was 230 ℃,and quadrupole temperature was 150 ℃;The detection mode was SIM mode;The detection ion(m/z)of methyl mesylate was 79,that of ethyl mesylate was 79,that of propyl mesylate was 109,and that of isopropyl mesylate was 123.Result:Under each ion channel,the blank solvent and blank auxiliary materials did not interfere with the detection of each solvent,the separation degree of each solvent was greater than 1.5.The results showed that the linear range of aryl sulfonates were good at 0.04～1.0 μg·mL-1,respectively.The correlation coefficient r＞0.990,the quantitative limit of each impurity was 0.02 ng,the detection limit was 0.01 ng,and the RSD of each impurity was less than 3.0％(n=6).Conclusion:The method has good precision and accuracy.It can be applied to the detection of sulfonate impurities in Lenvatinib Mesilate Capsules.
lenvatinib mesilate capsulessulfonate impuritiesgas chromatograph coupled with mass spectrometry detector(GC-MS)
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