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大体积进样法测定白酒中7种邻苯二甲酸酯

Determination of Seven Kinds of Phthalate Esters in White Spirit with Direct Sample Introduction in Large Volume

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【作者】 郭丽萍张丝柳杜小弟雷家珩

【Author】 Guo Li-ping;Zhang Si-liu;Du Xiao-di;Lei Jia-heng;Department of Chemistry,Wuhan University of Technology;

【机构】 武汉理工大学化学系

【摘要】 采用高效液相色谱大体积进样法测定白酒中7种邻苯二甲酸酯类物质。通过添加乙醇或水使试样基体的酒精度调整至38%vol,然后直接进样1 000μL,使用HC-C18色谱柱,以70%乙腈水溶液和纯乙腈为流动相梯度洗脱,以紫外检测器检测(波长225 nm)。DAP、BBP、DBP、DEHP和DNOP等5种目标物在0.02~2 mg/L浓度范围内具有良好的线性响应关系,检出限(S/N=3)为0.005~0.007 mg/kg;DINP、DIDP等2种目标物在0.1~4 mg/L浓度范围内具有良好的线性响应关系,检出限(S/N=3)为0.04~0.05 mg/kg。在高、中、低三种不同加标水平下,各目标物的回收率在87%~106%之间,相对标准偏差(n=6)均不超过7%。

【Abstract】 Seven kinds of phthalate esters in white spirit were determined with direct sample introduction in large volume by high performance liquid chromatography. Alcohol degree of the sample matrix was adjusted to 38%vol by adding ethanol or water, and sample was directly injected 1 000 μL with HC-C18 Column, gradient was eluted by 70% acetontrile-water and pure acetontrile was used as mobile phase and determined by UV detector(225 nm wavelength). A good linear response for target compounds of DAP, BBP, DBP, DEHP, DNOP, etc. could be obtained within the concentration of 0.02-2 mg/L with detection limit(S/N=3) of 0.005-0.007 mg/kg; A good linear response for target compounds of DINP, DIDP etc. also could be obtained within the concentration of 0.1-4 mg/L with detection limit(S/N=3) of 0.04-0.05 mg/kg. The recovery of each target compound at high, middle and low level of concentration ranged from 87% to 106%. The relative standard deviation(n=6) was less than 7%.

  • 【分类号】O657.72;TS262.3
  • 【被引频次】6
  • 【下载频次】134
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