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补充检验方法研究  

Study on the supplementary test method for naphthalene,diphenhydramine and lidocaine hydrochloride in nasal cold compress gel(dew)

作　　者：王跃 尹燕杰 WANG Yue;YIN Yan-jie(Harbin Center for Drug and Medical Device Testing,Harbin 150000,China)

机构地区：[1]哈尔滨市药品和医疗器械检验检测中心,哈尔滨150000

出　　处：《药物分析杂志》2024年第9期1624-1631,共8页Chinese Journal of Pharmaceutical Analysis

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 C_(18)(100 mm×2.1 mm,1.7μm)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10~200μg·mL^(-1)范围内,线性关系良好(r>0.9990)。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。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-triple 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 standard method and confirmed by HPLC-MS.The separation was performed on a XTerra RP18(150 mm×4.6 mm,5μm)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 C_(18)(100 mm×2.1 mm,1.7μm)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>0.9990).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).

关 键 词：鼻用冷敷凝胶(露) 盐酸萘甲唑啉 盐酸苯海拉明 盐酸利多卡因 高效液相色谱法 高效液相色谱串联质谱法 补充检验方法 

分 类 号：R917[医药卫生—药物分析学]