Accuracy profile理论在高效液相色谱法测定纺织品中3种有机溶剂残留中的应用
Application of Accuracy Profile Theory in HPLC Determination of 3 Organic Solvent Residues in Textiles
摘 要
样品经超纯水机械振荡萃取，提取液在Spursil C18色谱柱上分离，以甲醇-水-乙腈（25+70+5）混合液为流动相进行洗脱，检测波长为200 nm。N，N-二甲基甲酰胺、N，N-二甲基乙酰胺和N-甲基吡咯烷酮的质量浓度在0.5~10 mg·L-1内与峰面积呈线性关系，检出限（3S/N）为1.1~2.8 mg·kg-1，测定下限（10S/N）为3.7~9.3 mg·kg-1。采用Accuracy profile理论验证方法的准确性，并评估了测定的不确定度，说明方法可满足3种有机溶剂的日常检测要求。
Accuracy profile理论
N-甲基吡咯烷酮
N,N-二甲基甲酰胺
N,N-二甲基乙酰胺
纺织品
HPLC
Accuracy profile theory
N,N-dimethylacetamide
N,N-dimethylformamide
N-methyl-2-pyrrolidone
Textile
Abstract
After the sample was extracted by mechanical oscillation with ultrapure water, the extract was separated on a Spursil C18 chromatographic column with a mixture of methanol, water and acetonitrile (25+70+5) as mobile phase for elution. The detection wavelength was 200 nm. Linear relationships were found between the peak areas with the mass concentrations of N,N-dimethylformamide, N,N-dimethylacetamide and N-methyl-2-pyrrolidone in the range of 0.5-10 mg·L-1, with detection limits (3S/N) in the range of 1.1-2.8 mg·kg-1, and the lower limits of determination (10S/N) in the range of 3.7-9.3 mg·kg-1. The method accuracy was validated according to the Accuracy profile theory, and the measurement uncertainty was evaluated. Results showed that the method could meet the daily detection requirements of the 3 organic solvents.
中图分类号 O656.31 DOI 10.11973/lhjy-hx201703013
所属栏目 工作简报
基金项目 浙江省分析测试科技计划项目（2014C37089）；宁波出入境检验检疫局科技计划项目（甬K05-2015）；浙江理工大学开放式基金项目（2014KF08）
收稿日期 2016/2/11
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备注保琦蓓(1982-)女,贵州普安人,高级工程师,博士,研究方向为生态纺织品检测。E-mail:baoqibei@126.com
引用该论文: BAO Qi-bei,FU Ke-jie,QIAN Dan,REN Qing-qing. Application of Accuracy Profile Theory in HPLC Determination of 3 Organic Solvent Residues in Textiles[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(3): 309～314
保琦蓓,傅科杰,钱丹,任清庆. Accuracy profile理论在高效液相色谱法测定纺织品中3种有机溶剂残留中的应用[J]. 理化检验－化学分册, 2017, 53(3): 309～314
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【15】ZHANG X, ZHAO X, ZHANG C, et al. Accuracy profile theory for the validation of an LC-MS-MS method for the determination of risperidone and 9-hydroxyrisperidone in human plasma[J]. Chromatographia, 2010,71(11):1015-1023.
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