QuEChERS-高效液相色谱法快速测定稻谷和土壤中16种多环芳烃
Rapid Determination of 16 Polycyclic Aromatic Hydrocarbons in Rough Rice and Soil by QuEChERS-HPLC
摘 要
提出了同时测定稻谷和土壤中16种多环芳烃(PAHs)的QuEChERS-高效液相色谱法(HPLC)。优化的QuEChERS条件为:乙腈浸泡过夜,超声提取15 min,漩涡振荡2 min,再经盐析、脱水后,N-丙基乙二胺(PSA)、C18E填料吸附剂净化。样品净化液采用HPLC-FLD及HPLC-DAD进行分析。16种PAHs的质量浓度在一定范围内呈线性,检出限(3S/N)在0.20~2.0 μg·L-1之间。糙米、稻壳和土壤中16种PAHs的基质加标回收率分别在85.0%~106%,81.5%~103%,76.7%~103%之间,相对标准偏差(n=3)均小于7.5%。
高效液相色谱法
多环芳烃
稻谷
土壤
QuEChERS
HPLC
PAHs
Rough rice
Soil
Abstract
QuEChERS-HPLC was applied to the simultaneous determination of 16 polycyclic aromatic hydrocarbons (PAHs) in rough rice and soil. The optimal conditions for QuEChERS were as follows: the sample was soaked overnight in acetonitrile, and extracted ultrasonically with the same solvent for 15 min, and then swirled for 2 min. After salting out and dehydration, the extract was cleaned up with PSA and C18E, and the purified extract was analyzed by HPLC -FLD and HPLC-DAD. Linearity for the 16 PAHs were kept between definite mass concentration ranges. Values of detection limits (3S/N) for the 16 PAHs were found in the range of 0.20-2.00 μg·L-1.Recovery was tested by addition of standards to the respective matrixes, values of recovery found were in the ranges of 85.0%-106% for brown rice, 81.5%-103% for rice hull and 76.7%-103% for soil, with RSDs (n=3) less than 7.5%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201609005
所属栏目 工作简报
基金项目 地质大调查项目(12120113014800)
收稿日期 2015/12/25
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备注吕爱娟(1981-),女,江苏常州人,工程师,硕士,主要从事环境监测工作。
引用该论文: L Ai-juan,SHI Lei,CAI Xiao-hu,SHEN Jia-lin. Rapid Determination of 16 Polycyclic Aromatic Hydrocarbons in Rough Rice and Soil by QuEChERS-HPLC[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(9): 1017～1021
吕爱娟,时磊,蔡小虎,沈加林. QuEChERS-高效液相色谱法快速测定稻谷和土壤中16种多环芳烃[J]. 理化检验－化学分册, 2016, 52(9): 1017～1021
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参考文献
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【10】ALBINET A, TOMAZ S, LESTREMAU F. A really quick easy cheap effective rugged and safe (QuEChERS) extraction procedure for the analysis of particle-bound PAHs in ambient air and emission samples［J］. Science of the Total Environment, 2013(450/451):31-38.
【2】ANASTASSIADES M, LEHOTAY S J, STAJNBAHER D, et al. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce［J］. Journal of AOAC International, 2003,86(2):412-431.
【3】KAO T H, CHEN S, CHEN C J, et al. Evaluation of analysis of polycyclic aromatic hydrocarbons by the QuEChERS method and gas chromatography-mass spectrometry and their formation in poultry meat As affected by marinating and frying［J］. Journal of Agricultural and Food Chemistry, 2012,60(6):1380-1389.
【4】郭萌萌,吴海燕,杨帆,等.改进的QuEChERS-高效液相色谱法测定水产品中16种多环芳烃［J］.环境化学, 2013,32(6):1025-1031.
【5】张晓强,张波,方萍,等.QuEChERS-超高效液相色谱-串联质谱法快速测定鱼肉中22种磺胺类药物残留［J］.理化检验-化学分册, 2015,51(3):369-374.
【6】DANKYI E, GORDON C, CARBOO D, et al. Quantification of neonicotinoid insecticide residues in soils from cocoa plantations using a QuEChERS extraction procedure and LC-MS/MS［J］. Science of the Total Environment, 2014,499(1):276-283.
【7】赵洁,何强,姚秉华,等.改进QuEChERS-气相色谱-质谱法快速分析测定农用土壤中多环芳烃［J］.分析试验室, 2012,31(2):33-37.
【8】张萌萌,陈剑伟,于天祥,等.基质固相分散技术-气质联用法快速测定大米中的多环芳烃［J］.食品科技, 2014,39(1):327-330.
【9】沈小明,吕爱娟,沈加林.不同提取方法测定海洋沉积物中痕量PAHs的比较［J］.环境化学, 2010,29(6):1177-1178.
【10】ALBINET A, TOMAZ S, LESTREMAU F. A really quick easy cheap effective rugged and safe (QuEChERS) extraction procedure for the analysis of particle-bound PAHs in ambient air and emission samples［J］. Science of the Total Environment, 2013(450/451):31-38.
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