摘要
建立了高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定化妆品中9种二苯甲酮类紫外吸收剂含量的方法。将样品0.1 g用乙腈30 mL超声提取30 min,冷却至室温,稀释至50 mL,过滤,以C_(18)色谱柱为固定相,以不同体积比的乙腈和0.1%(体积分数)甲酸溶液的混合液为流动相进行梯度洗脱。质谱分析中采用电喷雾正离子源和多反应监测模式检测,外标法定量。结果表明:样品基质效应较小,可不予考虑。9种二苯甲酮类化合物的质量浓度均在0.50~500μg·L^(-1)内与其对应的响应值呈线性关系,检出限(3s/k)为0.022~0.652μg·L^(-1)。连续测定混合标准溶液,9种二苯甲酮类紫外吸收剂测定值的相对标准偏差(n=6)均小于5.0%。按标准加入法进行回收试验,测得回收率为70.9%~116%。按此方法分析了15批样品,2批检出二苯酮-3,检出量为1.53%和4.67%,1批检出二苯酮-10,检出量为0.00126%。
The method for simultaneous determination of the 9 benzophenones for ultraviolet absorber in cosmetics by high performance liquid chromatography-tandem mass spectrometry was established.The sample(0.1 g)was treated in 30 mL of acetonitrile by ultrasonic extraction for 30 min,cooled to room temperature,diluted to 50 mL and filtered.C_(18) chromatographic column was used as the stationary phase,and a mixture of acetonitrile and 0.1%(φ)formic acid aqueous solution at different volume ratios was used as the mobile phase for gradient elution.The electrospray ionization source(ESI;)and multiple reaction monitoring mode were adopted into mass spectrometry analysis,and external standard method was used for quantitative analysis.It was showed that the matrix effect of the sample was small and could be ignored.Linear relationships between mass concentrations of the 9 benzophenones and their response values were kept in the same range of 0.50-500μg·L^(-1),with detection limits(3s/k)in the range of 0.022-0.652μg·L^(-1).The mixed standard solution were determined,with RSDs(n=6)of the determined values less than 5.0%.Test for recovery was made by standard addition method,giving values of recovery in the range of 70.9%-116%.15 batches of samples were analyzed by this method,and benzophenone-3 was detected in 2 batches,with the detection amounts of 1.53%and 4.67%,and benzophenone-10 was detected in 1 batch,with the detection amount of 0.00126%.
作者
鲁素雅
邢海艳
刘洋
吴义春
金鹏
陈长毅
LU Suya;XING Haiyan;LIU Yang;WU Yichun;JIN Peng;CHEN Changyi(Huai′an Institute for Food and Drug Control,Huai′an 223005,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2021年第12期1104-1109,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词
高效液相色谱-串联质谱法
二苯甲酮类
紫外吸收剂
high performance liquid chromatography-tandem mass spectrometry
benzophenone
ultraviolet absorber
