摘要
目的:采用高效液相色谱串联飞行时间质谱法高通量筛查化妆品中的非法添加成分,并建立高效液相色谱串联三重四极杆质谱法测定化妆品中他克莫司和吡美莫司的方法。方法:通过高效液相色谱串联飞行时间高分辨质谱法对市售儿童化妆品进行风险物质高通量初步筛查,发现1批他克莫司阳性样品,然后运用高效液相色谱串联三重四极杆质谱法进行定性定量测定。经实验条件优化,以含17.5 mmol·L^(-1)乙酸-5 mmol·L^(-1)乙酸铵的水溶液(A)和含17.5 mmol·L^(-1)乙酸-5 mmol·L^(-1)乙酸铵的甲醇溶液(B)为流动相,采用Waters ACQUITY UPLC BEH C18色谱柱,进行梯度洗脱分离,柱温45℃,流速0.3 mL·min^(-1),然后经三重四极杆质谱正离子多反应监测模式扫描。结果:他克莫司和吡美莫司质量浓度在0.5~50 ng·mL^(-1)范围内线性关系良好,检出限均为10 ng·g^(-1),定量限均为25 ng·g^(-1)。在膏霜、乳液、水剂、油剂4种代表基质中各浓度水平加标回收率均在93.1%~110.7%,回收率良好。经测定,1批儿童化妆品中检出他克莫司,含量为2.8 mg·kg^(-1)。结论:该方法弥补了化妆品中非法添加的他克莫司及吡美莫司检验方法的缺失,为化妆品的日常监督监管提供了技术支持。
Objective:To establish a method for the determination of tacrolimus and pimeclimus in cosmetics by high performance liquid chromatography with a triple quadruple tandem mass spectrometry(HPLC-MS/MS),and was used to high-throughput screening for illegally added ingredients in cosmetics by high performance liquid chromatography-time-of-flight mass spectrometry(HPLC-Q TOF MS/MS).Methods:Through high-throughput screening of the initial risk assessment of children's cosmetics sold in markets by HPLC-Q TOF MS/MS,a batch of tacrolimus positive children's cosmetics was identified,and then a method was established for qualitative and quantitative determination by HPLC-MS/MS.After the optimization of chromatographic analysis conditions,the gradient elution was performed on a Waters ACQUITY UPLC BEH C_(18)column at 45℃,which were used an aqueous solution(containing 17.5 mmol·L^(-1)acetic acid-5 mmol·L^(-1)ammonium acetate)and a methanol solution(containing 17.5 mmol·L^(-1)acetic acid-5 mmol·L^(-1)ammonium acetate)as mobile phases at the flow rate of 0.3 mL·min^(-1).The analytes were scanned by HPLC-MS/MS in positive ion multiple reaction monitoring mode.Results:There was a good linear relationship between Tacrolimus and pimecrolimus in the concentration range of 0.5-50 ng·mL^(-1).The limits of detection were 10 ng·g^(-1)and the limits of quantification concentration were 25 ng·g^(-1).The spiked recoveries of each concentration level were good,which ranged from 93.1% to 110.7% in the four respective matrices,such as cream,emulsion,water and oil.Tacrolimus was detected in 1 batch of children's cosmeticsat 2.8 mg·kg^(-1).Conclusion:This method makes up for the lack of test methods for tacrolimus and pimecrolimus illegally addition in cosmetics,and provides technical supports for the daily supervision in cosmetics.
作者
牛水蛟
于海英
董亚蕾
王海燕
刘慧香
孙磊
李启艳
NIU Shui-jiao;YU Hai-ying;DONG Ya-lei;WANG Hai-yan;LIU Hui-xiang;SUN Lei;LI Qi-yan(NMPA Key Laboratory for Quality Control of Cosmetics Raw Material,Shandong Institute for Food and Drug Control,Jinan 250101,China;National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2023年第10期1759-1765,共7页
Chinese Journal of Pharmaceutical Analysis
