摘要
目的:建立同时测定外用制剂中咪康唑等13种抗真菌化学成分的UPLC-MS/MS法。方法:采用液质联用法,应用C 18柱,以0.1%甲酸溶液-0.1%甲酸乙腈溶液为流动相进行梯度洗脱,质谱采用正离子模式,多反应监测,流速为0.3mL·min^-1。结果:在相应的浓度范围内,13种抗真菌化学成分质量浓度与峰面积呈良好的线性关系(r≥0.99);在3个不同浓度加标水平下,平均回收率为87.4%~113.5%,RSD为1.1%~6.9%,各化学成分的检出限在0.003 mg·kg^-1~0.12 mg·kg^-1,收集的10批次样品中,1批次检出酮康唑和咪康唑,含量分别为0.2 mg·g^-1、11.3 mg·g^-1,1批次检出咪康唑和特比萘芬含量分别为10.9 mg·g^-1、2.0mg·g^-1,4批次检出咪康唑,含量分别为26.7 mg·g^-1、32.3 mg·g^-1、6.4 mg·g^-1、18.1mg·g^-1。结论:该法分析速度快,操作简便、快捷、灵敏度高、能准确可靠地测定外用制剂中非法添加抗真菌类化学成分的定性筛查和定量检测,可用于外用制剂的质量控制。
To establish a UPLC-MS/MS analytical method for the simultaneous analysis of 13 anti-fungal compounds in external preparation.Methods:The separation was performed on C18 column using a gradient elution acetonitrile(containing 0.1%formic acid)and 0.1%formic acid).A triple quadrupole mass spectrometer operating in positive electrospray ionization mode with multiple reaction monitoring was used with gradient elution at a flow rate of 0.30mL.min^-1.Results:13 anti-fungal compounds showed good linear relationships within their own rangers within their own ranges,the correlation coefficients(r)were above 0.99,Under three different concentration levels,their average recoveries ranged from 87.4%to 113.5%with the RSDs of 1.1%to 6.9%.The LODS were all in range of 0.003 mg·kg^-1~0.12 mg·kg^-1.Among the 10 batches of samples collected,ketoconazole and Miconazole were detected in one batch,with the content of 0.2 mg·g^-1 and 11.3 mg·g^-1,Miconazole and Terbinafine were detected in one batch,with the content of 10.9 mg·g^-1 and 2.0 mg·g^-1,Miconazole were detected in four batchs,with the content of 26.7 mg·g^-1、32.3 mg·g^-1、6.4 mg·g^-1、18.1mg·g^-1.Conclusion:the method not only is convenient,rapid,sensitive and accurate,but also can be used for the qualitative screening and quantitative determination of illegally added 13 anti-fungal compounds illegally added in external preparation.
作者
张艳萍
周宗洲
黄婉锋
张敏
何作民
钱鑫
关倩怡
Zhang Yanping;Zhou Zongzhou;Huang Wanfeng;Zhang Min;He Zuomin;Qian Xin;Guan Qianyi(FoShan Institute for Drug and Food Control,Guang Dong FoShan 528051;FoShan Center for Disease Control and Prevention,Guang Dong FoShan 528051)
出处
《北方药学》
2020年第9期25-30,共6页
Journal of North Pharmacy
基金
佛山市医学类科技公关项目中药制剂中非法添加咪康唑等24种抗真菌类药物的UPLC-MS/MS方法研究与应用。
