Determination of 18 Polycyclic Aromatic Hydrocarbons in PM2.5 by Liquid Chromatography with Accelerated Solvent Extraction
摘 要
提出了加速溶剂萃取-液相色谱法测定德国GS标志认证的18种多环芳烃(PAHs)的方法。PM2.5样品经二氯甲烷-丙酮(1+1)混合液在100℃加速溶剂萃取5 min,循环2次。萃取液浓缩至约1 mL,氮吹至近干,用乙腈定容至1 mL。所得溶液以不同体积比的乙腈和水的混合液为流动相进行梯度洗脱,采用紫外检测器(UV)-荧光检测器(FLD)串联检测,其中UV (波长254 nm)测定苊烯,FLD两个波长通道分别测定苯并[j]荧蒽和其余16种PAHs。结果表明:18种PAHs的质量浓度均在0.02~1.00 mg·L-1内与对应的峰面积呈线性关系,检出限(3S/N)为0.005~0.018 mg·L-1。按标准加入法进行回收试验,回收率为83.3%~108%,测定值的相对标准偏差(n=5)为0.82%~5.2%。
Abstract
A method was proposed for determination of 18 polycyclic aromatic hydrocarbons (PAHs) identified by GS in Germany by liquid chromatography (LC) with accelerated solvent extraction (ASE). The PM2.5 sample was extracted by ASE with a mixture of dichloromethane-acetone (1+1) at 100℃ for 5 min, with 2 cycle. The extract was concentrated to about 1 mL, then to near dryness by N2-blowing, and the residue was made its volume up to 1 mL with acetonitrile. The solution obtained was analyzed with ultraviolet (UV)-fluorescence (FLD) detector, with the mixture of acetonitrile and water in different volume ratios as mobile phase for gradient elution. Acenaphthylene (AcPy) was detected by UV (λ=254 nm), and benzo[j] fluoranthene (BkF) and the other 16 PAHs were respectively determined by two wavelength channels of FLD. As shown by the results, linear relationships between values of peak area and mass concentration of 18 PAHs were found in the same range of 0.02-1.00 mg·L-1, and detection limits (3S/N) ranged from 0.005 to 0.018 mg·L-1. Test for recovery was made by standard addition method, giving results in the range of 83.3%-108%, and RSDs (n=5) ranged from 0.82% to 5.2%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201810005
所属栏目 工作简报
基金项目 国家自然科学基金项目(411050116);中央高校基本科研业务费专项资金项目(2652015332)
收稿日期 2017/10/29
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备注魏沙沙,硕士研究生,从事环境分析化学方面的研究
引用该论文: WEI Shasha,CHEN Jinchao,ZHANG Wan,RAO Mengnan,FENG Tiantian,DONG Xueling. Determination of 18 Polycyclic Aromatic Hydrocarbons in PM2.5 by Liquid Chromatography with Accelerated Solvent Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(10): 1142~1148
魏沙沙,陈锦超,张婉,饶梦囡,冯甜甜,董雪玲. 加速溶剂萃取-液相色谱法测定PM2.5中18种多环芳烃[J]. 理化检验-化学分册, 2018, 54(10): 1142~1148
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参考文献
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【2】KIM K H, JAHAN S A, KABIR E, et al. A review of airborne polycyclic aromatic hydrocarbons (PAHs) and their human health effects[J]. Environment International, 2013,60:71-80.
【3】SALADI R, AUSTIN L, GAO D, et al. The combination of benzo[a]pyrene and ultraviolet A causes an in vivo time-related accumulation of DNA damage in mouse skin[J]. Photochemistry & Photobiology, 2003,77(4):413-419.
【4】TCHOU-WONG K M, JIANG Y, YEE H, et al. Lung-specific expression of dominant-negative mutant p53 in transgenic mice increases spontaneous and benzo(a)pyrene-induced lung cancer[J]. American Journal of Respiratory Cell & Molecular Biology, 2002,27(2):186-193.
【5】姜国红,高华,伦立民.结肠癌和肝癌与多环芳烃类致癌物的相关性[J].齐鲁医学杂志, 2015(5):524-526.
【6】高少鹏,刘大锰,安祥华,等.高效液相色谱法测定某钢铁厂地区大气颗粒物PM2.5中16种多环芳烃[J].环境科学, 2006,27(6):1052-1055.
【7】王宏菊,刘丽,刘志红,等.高效液相色谱法测定橡胶及其制品中16种多环芳烃[J].理化检验-化学分册, 2009,45(5):546-548.
【8】SAMARA C, LINTELMANN J, KETTRUP A. Determination of selected polynuclear aromatic hydrocarbons in waste water and sludge samples by HPLC with fluorescence detection[J]. Toxicological & Environmental Chemistry Reviews, 2008,48(1/2):89-102.
【9】SARRAZIN L, CATHERINE D, EMMANUEL W, et al. Determination of polycyclic aromatic hydrocarbons (PAHs) in marine, brackish, and river sediments by HPLC, following ultrasonic extraction[J]. Journal of Liquid Chromatography & Related Technologies, 2006,29(1):69-85.
【10】陈艳,李永波,何丰瑞,等.超声萃取-高效液相色谱法同时测定大气PM2.5中16种多环芳烃(PAHs)[J].中国卫生检验杂志, 2014(22):3217-3220.
【11】杨坪,龚必辅,熊英,等.大气颗粒物中多环芳烃的索氏提取研究[J].中国环境监测, 1999,15(6):16-20.
【12】牟世芬,刘克纳,阎炎,等.加速溶剂萃取技术及其在环境分析中的应用[J].环境化学,1997,16(4):387-391.
【13】房丽萍,邱赫男,王伟,等.土壤和沉积物中多环芳烃分析技术研究进展[J].理化检验-化学分册, 2015,51(9):1339-1346.
【14】祝本琼,陈浩,李胜清.基于轻质萃取剂的溶剂去乳化分散液-液微萃取-气相色谱法测定水样中多环芳烃[J].色谱, 2012,30(2):201-206.
【15】游钒,刘滔,曹霞,等.大气PM2.5中16种多环芳烃的聚焦微波辅助萃取-气相色谱质谱联用快速测定法[J].环境与健康杂志, 2017(11):999-1003.
【16】白珊,欧阳振中,罗道成.高效液相色谱法测定煤沥青中16种多环芳烃[J].分析试验室, 2016(9):1078-1082.
【17】那广水,刘春阳,张琳,等.固相膜萃取-超高效液相色谱-荧光法测定极地水体中多环芳烃[J].分析试验室, 2011,30(1):29-31.
【18】江阳,刘滔,汪文家,等.加速溶剂萃取-高效液相色谱法同时测定大气颗粒物PM2.5中16种多环芳烃[J].中国测试, 2015,41(6):43-46.
【19】黄东勤,王盛才,陈一清,等.加速溶剂萃取-高效液相色谱法测定土壤中16种多环芳烃[J].中国环境监测, 2008,24(3):26-29.
【20】史纯珍,屈瑶,毛旭.大气细颗粒物(PM2.5)中多环芳烃的分析测定与污染特征[J].环境化学, 2015,34(8):1417-1423.
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