高效液相色谱-串联质谱法测定天然彩色棉中23种邻苯二甲酸酯  

HPLC-MS/MS Determination of 23 Phthalate Esters in Naturally Colored Cotton

作　　者：王晓娟[1] 桂家祥 林振兴[1] 杨力生[1] 

机构地区：[1]宁波出入境检验检疫局,宁波315012 [2]赣州出入境检验检疫局,赣州332000

出　　处：《理化检验（化学分册）》2017年第11期1265-1270,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家质检总局科技计划项目(2015IK183;2016IK171);宁波市自然科学基金(2014A610116)

摘　　要：采用高效液相色谱-串联质谱法测定天然彩色棉中23种邻苯二甲酸酯的含量。天然彩色棉样品经破碎后,称取粉末1.000 0g,用甲醇30mL超声提取30min。提取液蒸馏浓缩并用氮气吹至近干,用甲醇定容至1mL,经0.45μm有机过滤膜过滤后,以Kinetex-C_(18)色谱柱为分离柱,以不同体积比的甲醇和0.1%(体积分数)甲酸溶液为流动相进行梯度洗脱,采用电喷雾正离子源多反应监测模式检测。23种邻苯二甲酸酯的质量浓度均在0.01~0.50mg·L^(-1)内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.01~4.05μg·kg^(-1)。以空白样品为基体进行加标回收试验,所得回收率为85.2%~105%,测定值的相对标准偏差(n=6)为0.60%~12%。HPLC-MS/MS was applied to the determination of 23 phthalate esters in naturally colored cotton.The sample of naturally colored cotton was crushed,and then 1.000 0 g of powder weighed was extracted ultrasonically with 30 mL of methanol for 30 min.The extract was concentrated by distillation and blown to near dry with nitrogen.The residue was taken up with methanol and diluted to 1 mL with methanol.The solution was filtered on 0.45μm organic filtering membrane.Kinetex-C_（18） chromatographic column was used as stationary phase,and the mixture of methanol and 0.1%（φ）formic acid solution mixed in different ratios was used as mobile phase in gradient elution.ESI＋and multi-reactions monitor mode were adopted in MS/MS.Linear relationships between values of peak area and mass concentration of the 23 phthalate esters were kept in the same range of 0.01-0.50 mg·L^（-1）,with detection limits（3 S/N）in the range of 0.01-4.05μg·kg^（-1）.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 85.2%-105%,with RSD′s（n=6）in the range of 0.60%-12%.

关 键 词：高效液相色谱-串联质谱法 天然彩色棉 邻苯二甲酸酯 

分 类 号：O657.63[理学—分析化学]