RESUMO
OBJECTIVE:To establish a method for the residual simultaneous determination of methanol,alcohol,dichlorometh-ane,n-hexane,tetrahydrofuran and benzene in tosufloxacin tosylat. METHODS:Headspace GC was performed on the capillary col-umn with 6%cyanopropylphenyl-94%dimethylpolysiloxane(DB-624)as fixative lipid,temperature programmed,the inlet temper-ature was 180 ℃,detector was flame ionization detector with temperature of 300 ℃,carrier gas was high purity N2 at a flow rate of 1.5 mL/min,split ratio was 10:1,headspace equilibrium temperature was 100℃,equilibrium time was 40 min,headspace sam-ple volume was 10 mL,and the headspace sample volume was 1 mL. RESULTS:The linear range was 178.3-1782.7 μg/mL for methanol (r=0.9991),301.2-3012.1 μg/mL for alcohol(r=0.9997),33.81-338.10 μg/mL for dichloromethane(r=0.9993), 18.02-180.22 μg/mL for n-hexane(r=0.9991),43.26-432.58 μg/mL for tetrahydrofuran(r=0.9991)and 0.1268-1.2681 μg/mL for benzene(r=0.9991);limits of quantification were 0.31,3.00,0.67,0.02,0.005,0.10 μg/mL,limits of detection were 0.15, 1.51,0.22,0.01,0.001,0.05 μg/mL;RSD of precision test was no higher than 3.1%;RSDs of methanol and n-hexane in stabili-ty and reproducibility tests were no higher than 5%;recoveries were 93.72%-102.20%(RSD=3.1%,n=9),90.10%-101.79%(RSD=4.0%,n=9),97.07%-103.11%(RSD=2.0%,n=9),92.38%-103.83%(RSD=3.9%,n=9),95.44%-103.62%(RSD=2.8%,n=9),and 94.00%-104.73%(RSD=4.1%,n=9). CONCLUSIONS:The method is rapid,sensitive,accurate,and suitable for the residual determination of methanol,alcohol,dichloromethane,n-hexane,tetrahydrofuran and benzene in tosufloxacin tosylat.
RESUMO
Objective:To establish an HPLC method for the determination of patulin in health foods containing hawthorn to im-prove the quality control of patulin in related health foods. Methods:An Agilent TC-C18(2)(250 mm ×4.6 mm, 5 μm) column was used with the temperature of 30℃. The mobile phase consisted of 0. 8% tetrahydrofuran and the flow rate was 1. 0 ml·min-1 . The detection wavelength was set at 276nm. Results:The calibration curve of patulin was linear within the range of 1-20ng(r=1. 000 0), the average recovery was 92. 1% and RSD was 2. 2%(n=6). Conclusion:The method is simple, reliable and accurate, which can be used in the content determination of patulin in health foods containing hawthorn.