Study on the supplementary test method for naphthalene,diphenhydramine and lidocaine hydrochloride in nasal cold compress gel(dew)
Objective:To develop an HPLC method for determination of naphazoline hydrochloride,diphenhydram hydrochloride and lidocaine hydrochloride added in nasal cold compress gel(dew),and to establish an HPLC-tri-ple quadrupole mass spectrometry(HPLC-MS)method to confirm the positive samples.Methods:The samples were extracted with acetonitrile,detected by high performance liquidchromatography,quantified by external stand-ard method and confirmed by HPLC-MS.The separation was performed on a XTerra RP18(150 mm x4.6 mm,5 μm)column with the mobile phase consisting of 50 mmol·L-1 ammonium acetate(the pH value was adjusted to 7.8 with acetic acid or ammonia solution)-acetonitrile(72:28)at the flow rate of 1.0 mL·min-1 and the detection wavelength was 230 nm.The analysis was performed on a BEH C18(100 mm × 2.1 mm,1.7 μm)column with a gradient elution of 0.1％formic acid aqueous solution-0.1％formic acid acetonitrile solution.The column temperature was set at 40 ℃ and the flow rate was 0.4 mL·min-1.Electrospray ionization source was applied and operated in positive electrospray ionization and the multiple reaction monitoring mode.Results:The method showed the lowest detection concentrations of naphthazoline hydrochloride,diphenhydramine hydrochloride and lidocaine hydrochloride were 2.4 ng·mL-1,50 ng·mL-1 and 50 ng·mL-1.The sample recoveries ranged from 93.9％to 104.6％.Good linearities were found in the concentration range of 10-200μg·mL-1(r＞0.999 0).A total of 42 batches of samples were detected and the total positive rate was 70％(36/42).Naphthazoline hydrochloride were found in 34 batches.Diphenhydramine hydrochloride and lidocaine hydrochloride were found in 2 batches simultaneously.Conclusion:The established method is specific,sensitive,simple,accurate and reliable.It can be used for the qualitative and quantitative determination of naphthazoline hydrochloride,diphenhydramine hydrochloride and lidocaine hydrochloride in nasal cold compress gel(dew).
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