摘要
目的:建立HPLC方法检测鼻用冷敷凝胶(露)中添加的盐酸萘甲唑啉、盐酸苯海拉明及盐酸利多卡因3个化学药物.建立HPLC-MS/MS法对检出的阳性样品进行确认.方法:试样采用乙腈提取后,用HPLC法检测,采用外标法定量,考察试验方法学,对市售样品进行检测.对阳性样品采用HPLC-MS/MS法确证.HPLC方法:采用XTerra RP18(150 mm×4.6 mm,5μm)色谱柱,以50 mmol·L-1乙酸铵(用乙酸或氨试液调节pH至7.8)-乙腈(72:28)为流动相,流速1.0 mL·min-1,检测波长230 nm;LC-MS/MS方法:采用BEH C18(100 mm×2.1 mm,1.7 μm)色谱柱,以0.1％甲酸水溶液-0.1％甲酸乙腈溶液为流动相,梯度洗脱,柱温40 ℃,流速0.4 mL·min-1;电喷雾电离源(ESI),正离子模式下多反应监测(MRM).结果:方法学考察试验表明,盐酸萘甲唑啉、盐酸苯海拉明和盐酸利多卡因的检测限分别为2.4、50和50 ng·mL-1,回收率为 93.9％～104.6％,在 10～200 μg·mL-1 范围内,线性关系良好(r＞0.999 0).对市售的42批样品进行检测,总体检出率达70％(36/42),其中34批检出盐酸萘甲唑啉,2批同时检出盐酸苯海拉明和盐酸利多卡因,存在较大的安全风险.结论:方法专属性强,灵敏度高,操作简单,准确可靠,可用于鼻用冷敷凝胶(露)中盐酸萘甲唑啉、盐酸苯海拉明及盐酸利多卡因的定性及定量检测.
Abstract
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).
维普
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