摘要
目的建立高效液相色谱法测定抑汗除臭类化妆品中阿托品、东莨菪碱和山莨菪碱的方法。方法样品经甲醇超声提取,采用C18色谱柱(250 mm×4.6 mm,5μm)分离后,以乙腈-20 mmol/L磷酸二氢钠为流动相梯度洗脱,采用二极管阵列检测器进行检测,以保留时间定性,外标法定量。结果在优化后的实验条件下,抑汗除臭类化妆品中阿托品、东莨菪碱和山莨菪碱得到有效分离,在1 mg/L~100 mg/L内线性相关系数r>0.999,方法检出限和定量限分别为3 mg/kg和10 mg/kg。3种托品烷类生物碱在10 mg/kg、50 mg/kg、200 mg/kg 3个浓度的加标量下,回收率为96.7%~108.2%(n=6),相对标准偏差为0.5%~4.5%。方法精密度、稳定性及重复性良好。结论本法准确、灵敏、前处理简单,可用于抑汗除臭类化妆品中阿托品、东莨菪碱和山莨菪碱的定量测定。
Objective This paper aims to establish a high-performance liquid chromatography method for the determination of atropine,scopolamine and anisodamine in antiperspirant and deodorant cosmetics.Methods The analytes in samples were ultrasonically extracted with methanol and then separated on a C18 column(250 mm×4.6 mm,5μm)with the mobile phase of acetonitrile-20 mmol/l phosphate buffer solution in gradient elution and detected by diode array detector.Qualitative analysis was done by retention time and quantitative analysis by external standard curves.Results Under optimized experimental conditions,atropine,scopolamine and anisodamine were effectively separated in antiperspirant and deodorant cosmetics.The method had good linearity within 1 mg/L-100 mg/L,with correlation coefficients(r)greater than 0.999.The limit of detection(LODs)and limit of quantitation(LOQs)were 3 mg/kg and 10 mg/kg,respectively.The average recoveries for the tropane alkaloids spiked at levels of 10 mg/kg,50 mg/kg,200 mg/kg were within 96.7%-108.2%,with relative standard deviations(RSDs)between 0.5%and 4.5%(n=6).The method showed good precision,stability and repeatability.Conclusion The developed method is accurate,sensitive and simple and can be applied for the determination of anisodamine,scopolamine and atropine in antiperspirant and deodorant cosmetics.
作者
严俊
YAN Jun(Hangzhou Municipal Center for Disease Control and Prevention,Zhejiang 310021,China)
出处
《中国卫生检验杂志》
CAS
2023年第20期2466-2468,共3页
Chinese Journal of Health Laboratory Technology
关键词
阿托品
东莨菪碱
山莨菪碱
M受体拮抗剂
高效液相色谱法
Atropine
Scopolamine
Anisodamine
M acetylcholine receptor antagonists
High performance liquid chromatography