摘要
建立了超高效液相色谱-三重四极杆质谱法(UPLC-MS/MS)快速筛查和准确定量按摩凝胶中对乙酰氨基酚、氨基比林、泼尼松、氢化可的松、酮洛芬、萘普生、双氯芬酸钠7种非法添加抗炎镇痛药和合成辣椒素。样品经甲醇超声提取,以5 mmol/L乙酸铵的水溶液-甲醇作为流动相,使用Agilent ZOBAX Eclipse Plus C18(3.0 mm×50 mm,1.8μm)色谱柱进行梯度分离,采用电喷雾离子源(正负离子模式),以多反应监测(MRM)模式检测,外标法定量。结果表明,在0.0050~0.40 mg/L的浓度范围内,各目标化合物的性关系良好(r>0.999),检出限为0.0003~0.001 mg/L,定量限为0.001~0.004 mg/L,在低、中、高3个加标水平下的平均回收率在90.9%~116.7%,相对标准偏差在0.8%~4.1%(n=5)。该方法样品前处理操作简单、快速,方法灵敏度高、准确度和精密度好,适用于按摩凝胶中7种非法添加抗炎镇痛药和合成辣椒素的快速筛查和定量。
A method of ultra-performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS)was established to rapidly screen and accurately quantify of 7 illegally added anti-inflammatory analgesics(namely paracetamol,aminopyrine,prednisone,hydrocortisone,ketoprofen,naproxen,and diclofenac sodium)and nonivamide in massage gel.The samples were ultrasonically extracted by methanol and analyzed on an Agilent ZORBAX Eclipse Plus C18(3.0 mm×50 mm×1.8μm-micron)column by gradient elution,using 5 mmol/L ammonium acetate aqueous-methanol as the mobile phase.Electrospray ion source(negative and positive ion mode)and multiple reaction monitoring(MRM)mode were used for MS detection.Meanwhile,the analytes were quantified by external standard method,and the results show that there are good linear relationships for the target compounds in the range from 0.0050 to 0.40 mg/L,with the correlation coefficients(r)greater than 0.999.The limits of detection(LOD)and the limits of quantitation(LOQ)of the method are in the ranges of 0.0003~0.001 mg/L and 0.001~0.004 mg/L,respectively.At three spiked levels,the recoveries for the target compounds are 90.9%~116.7%,with the relative standard deviations(RSD)of 0.8%~4.1%(n=5).This method is simple,rapid,high sensitivity,accurate and precise,which is suitable to rapidly screen and accurately quantify of 7 illegally added anti-inflammatory analgesics and nonivamide in massage gel.
作者
曾航日
钟菲菲
周鹏
李菁
涂林锋
ZENG Hangri;ZHONG Feifei;ZHOU Peng;LI Jing;TU Linfeng(Changsha Institute for Food and Drug Control,Changsha,Hunan 410000,China)
出处
《日用化学品科学》
2025年第1期51-55,共5页
Detergent & Cosmetics
关键词
超高效液相色谱-三重四极杆质谱
非法添加
合成辣椒素
按摩凝胶
ultra-performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS)
illegal additions
nonivamide
massage gel
作者简介
第一作者:曾航日(1989-),女,湖南人,工程师,硕士;通讯作者:周鹏,高级工程师,硕士,zhoupeng58@hnu.edu.cn。
