快速提取-超高效液相色谱法测定唇膏中11种酞酸酯
周江,季倩祎,余妙琴,杨浩,吴重彬
义乌市产品(商品)质量监督检验研究院,浙江义乌 322000
Determination of 11 kind of Phthalate Esters in Lipstick by Rapid Extraction and Ultra-Performance Liquid Chromatography
周江,季倩祎,余妙琴,杨浩,吴重彬
Yiwu Product (Commodity) Quality Supervision and Test Institute, Yiwu 322000, China
摘要:建立快速提取 -超高效液相色谱法测定唇膏中 11 种酞酸酯的检测方法。将唇膏样品涂覆在定量滤纸 上,用甲醇涡旋超声提取,色谱柱采用 Waters ACQUITY UPLC BEH C18 柱 (100 mm×2.1 mm,1.7 μm),流动相为乙 腈 -水,梯度洗脱,流量为 0.5 mL/min,用 PDA 检测器检测,检测波长 225 nm。以 3 倍空白噪音计,邻苯二甲酸二 甲酯 (DMP)、邻苯二甲酸二乙酯 (DEP) 的检出限分别为 1,2 mg/kg ;邻苯二甲酸二丙酯 (DPRP)、邻苯二甲酸二丁酯 (DBP)、邻苯二甲酸二戊酯 (DPP)、邻苯二甲酸二己酯 (DHXP)、邻苯二甲酸丁基苄基酯 (BBP)、邻苯二甲酸二 (2-乙基 ) 己酯 (DEHP)、邻苯二甲酸二正辛酯 (DNOP) 的检出限为 3 mg/kg ;邻苯二甲酸二异壬酯 (DINP)、邻苯二甲酸二异癸 酯 (DIDP) 的检出限为 30 mg/kg。方法的加标回收率为 86.6%~98.6%,测定结果的相对标准偏差为 0.6%~6.0%(n=6)。 该方法样品处理简单,提取效率高,分离效果好且灵敏度高,结合色谱图和紫外光谱图,能快速准确测定唇膏中 11 种 酞酸酯。
Abstract:A rapid extraction and ultra-performance liquid chromatography method was established for determining 11 kind of phthalate esters(PAEs) in lipstick. The lipstick sample was directly coated on the quantitative filter paper, and extracted by methanol using shaker and ultrasonic bath. PAEs were separated on Waters ACQUITY UPLC BEH C18 column(100 mm×2.1 mm, 1.7 μm) by gradient elution using acetonitrile-water as the mobile phase at a flow rate of 0.5 mL/min, and detected by PDA detector on detecting wavelength of 225 nm. The detection limits(S/N=3) of dimethyl phthalate and diethyl phthalate were 1 mg/kg and 2 mg/kg, respectively; the detection limits of dipropyl phthalate, dibutyl phthalate, dipentyl phthalate, dihexyl phthalate, benzyl butyl phthalate, bis(2-ethylhexyl) phthalate and di-n-octyl phthalate were 3 mg/kg; the detection limits of di-iso-nonyl phthalate and di-iso-decyl phthalate were 30 mg/kg. The average recoveries for PAEs in lipstick were 86.6%-98.6%. The relative standard deviations of determination results were 0.6%-6.0%(n=6). The pretreatment is simple, the extraction efficiency is high, and the separation is quick and effective. The method can satisfactory for determination of the 11 phthalate esters in lipstick.
关键词:唇膏;酞酸酯;超高效液相色谱法;定量滤纸
Keywords:lipstick; phthalate esters; ultra-performance liquid chromatography; quantitative filter paper
本文引用格式:
周江,季倩祎,余妙琴,等.快速提取-超高效液相色谱法测定唇膏中11种酞酸酯[J].化学分析计量,2016,25(3):77-80.
ZHOU J,JI Q Y,YU M Q,.Determination of 11 kind of Phthalate Esters in Lipstick by Rapid Extraction and Ultra-Performance Liquid Chromatography[J]. Chemical analysis and meterage,2016,25(3):77-80.
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