Advance of stir bar sorptive extraction

作为一种新型的环境友好型样品前处理技术,搅拌棒固相萃取(SbSE)集萃取、净化和富集为一体,已经在环境监测、食品安全和生物分析等领域进行了广泛应用。本文结合作者所在研究小组的研究工作,对近几年来SbSE技术的发展进行综述,重点阐述了各种新涂层的研究和应用,同时就SbSE发展方向提出了展望。Stir bar sorptive extraction(SBSE) is an environmentally-friendly technology of sample preparation which combines extraction,cleanup and enrichment together,and it has been developed rapidly and widely applied to the trace enrichment of various target analytes in environmental,food and biological samples.Based on our research,the advance of SBSE,especially,the development of new coatings,are review ed.At the same time,the possible development orientations of SBSE are discussed.国家自然科学基金项目(21077085);福建省自然科学基金项目(2010J01047

Determination of nitrofuran residues in feed and water samples by monolith-based stir bar sorptive extraction and high performance liquid chromatography

利用自制的以聚(乙烯基咪唑-二乙烯基苯)(VIdb)整体材料为涂层的固相萃取搅拌棒(VIdb-SbSE)萃取3种硝基呋喃类药物,然后与高效液相色谱-二极管阵列检测器联用建立了测定饲料和水样品中硝基呋喃类药物残留的方法。详细考察了萃取过程中萃取和解吸时间、样品基质的PH值以及离子强度等实验条件对萃取效率的影响。在最佳条件下,呋喃唑酮的线性范围为0.5~200μg/l,呋喃妥因和呋喃西林的线性范围为0.25~200μg/l,3种目标物的检出限(lO d)(S/n=3)在0.068~0.11μg/l之间,所建方法具有理想的日内和日间重现性(r Sd值均小于6%)。在对饲料和实际水样的测定中,不同加标浓度呋喃唑酮、呋喃妥因和呋喃西林的回收率在80.6%~108%之间。研究表明,所建立的方法具有简便、灵敏、环境友好等特点。A simple,efficient and sensitive method for the simultaneous determination of nitrofurantoin( NFT),furazolidone( FZD) and nitrofurazone( NFZ) in feed and water samples was developed by stir bar sorptive extraction( SBSE) coupled to high performance liquid chromatography w ith diode array detection.T he SBSE based on poly( vinylimidazole-divinylbenzene)( VIDB) monolithic material as coating w as used to concentrate the three target analytes.T o obtain the optimum extraction performance, several VIDB-SBSE parameters w ere investigated and studied,including pH value,ionic strength of sample matrix,extraction and desorption time.U nder the optimized experimental conditions,the linear ranges w ere 0.5- 200 μg / L for FZ D,0.25- 200 μg / L for N FT and N FZ.T he limits of detection( S / N = 3) w ere in the range of 0.068- 0.11 μg / L for the three analytes.T he precision of the proposed method w as evaluated in terms of intra- and inter-day repeatability calculated as R SD,and it w as found that the R SDs w ere all below 6%.T he developed method w as successfully applied to the determination of nitrofuran residues in animal feed and w ater samples.T he satisfactory recoveries of the spiked target compounds w ere in the range of 80.6%- 108%.国家自然科学基金项目(21377105;21077085); 福建省新世纪优秀人才项

Distribution of dimethylsulfide of Xiamen sea surface water in spring

采用固相微萃取(SPME) 气相色谱法(GC)测定了厦门海域20个站位表层海水中DMS二甲基硫的含量,并对其分布进行分析。结果表明,厦门海域DMS含量在0 65～40 69nmol·L-1,平均浓度为12 83nmol·L-1。其中,西海域的含量最高,东海域次之,同安湾最低。与其它海域海水中DMS浓度比较,厦门海域DMS含量较高,浓度变化范围大,与叶绿素a浓度及表层水温、盐度之间无明显的相关关系。Dimethylsulfide (DMS) in surface seawater samples collected at 20 stations in the Xiamen sea area were analyzed with SPME-GC method. The results showed that the DMS concentrations varied from 0.65 to 40.69 nmol·L~(-1) with an average of 12.83 nmol·L~(-1). The concentration was the highest in Xiamen Western sea area, while was lower in Eastern sea area and the lowest in Tong'an Bay. Comparation with other sea areas, DMS concentration in Xiamen sea was higher, with the large variation. There were no clear relationships DMS with chlorophyll a, temperature and salty in Xiamen sea.国家自然科学基金(20077022);; 教育部重点课题(教技司2000第156号

A new anionic exchange stir bar sorptive extraction coating based on monolithic material for the extraction of inorganic anion

A novel anionic exchange stir bar sorptive extraction (SBSE) coating based on poly(2(methacryloyloxy)ethyltrimethylammonium chloride-co-divinylbenzene) monolithic material for the extraction of inorganic anion was prepared. The effect of preparation conditions such as ratio of functional monomer to cross-linker, content of porogenic solvent on the extraction efficiencies were investigated in detailed. The monolithic material was characterized by elemental analysis, scanning electron microscopy and infrared spectroscopy. In order to investigate the extraction capacity of the new coating for inorganic anion, the new SBSE was combined with ionic chromatography with conductivity detection, Br-, NO3-, PO43- and SO42- were selected as detected solutes. Several extractive parameters, including pH value and ionic strength in sample matrix, desorption solvent, extraction and desorption time were optimized. The results showed that strongly ionic strength did not favor the extraction of anlaytes. Under the optimum experimental conditions, low detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target anions were achieved within the range of 0.92-2.62 and 3.03-9.25 mu g/L, respectively. The method also showed good linearity, simplicity, practicality and low cost for the extraction inorganic anions. Finally, the proposed method was successfully used to detect the two different trademarks of commercial purified water with satisfactory recovery in the range of 70.0-92.6%. To the best of our knowledge, this is the first to use SBSE to enrich inorganic anions. (C) 2010 Elsevier By. All rights reserved.National Nature Science Foundation of China [20805039]; Youth Talent Foundation of Fujian Province [2006F3117]; Start-up foundation of Xiamen University ; Innovation Foundation of Xiamen University [XDKJCX20063007

Determination of formaldehyde and phenol in waste water with static headspace-GC-FID

建立了静态顶空取样、气相色谱直接分析水样中甲醛和苯酚的方法。该方法有良好的重现性 ,甲醛、苯酚连续测定 6次的相对标准偏差分别为 1.9%和 4.7%。甲醛、苯酚的检测限分别为 0 .5 0 mg/m L和 0 .3 0 mg/m L。方法简便、快速、基底干扰小 ,适用于工业废水中甲醛和苯酚的同时、快速测定A method for determination of formaldehyde and phenol in waste water with static headspace GC FID has been developed. The detection limits for formaldehyde and phenol were 0.50 mg/mL and 0.30 mg/mL, respectively. The relative standard devirations tere 1.9% and 4.7% for those, respectively. The method has been proved to be simple, fast, matrix interference free, and can be used for the fast determination of formaldehyde and phenol in industrial waste water.福建省自然科学基金重点资助项目 (D0 0 2 -0 0 0 2 );; 教育部骨干教师资助计划 (2 0 0 0年

Preparation of cation-exchange stir bar sorptive extraction based on monolithic material and its application to the analysis of soluble cations in milk by ion chromatography

In this study, a new cation-exchange coating for stir bar sorptive extraction (SBSE) based on poly (acrylic acid-ethylene dimethacrylate) monolithic material was synthesized. The effect of polymerization conditions such as the ratio of functional monomer to cross-linker and the content of porogenic solvent on the extraction efficiencies were investigated in detail. The monolithic material was characterized by elemental analysis, scanning electron microscopy and infrared spectroscopy. In order to evaluate the usability of the new coating for the extraction of inorganic cations, the analysis of soluble K(+), Mg(2+) and Ca(2+) in milk by ion chromatography with conductivity detection was selected as a paradigm. Several extractive parameters, including pH value in sample matrix, desorption solvent, extraction and desorption time were optimized. Under the optimum conditions, low detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target cations were achieved within the range of 0.12-0.28 and 0.4-0.92 mu g L(-1), respectively. The method also showed good linearity, simplicity, practicality and low cost for the extraction of inorganic cations. Finally, the proposed method was successfully used to analyse three different trademarks of commercial milk samples with satisfactory recoveries in the range of 71.1% to 102.8%.National Nature Science Foundation of China[21077085]; Nature Science Foundation of Fujian Province of China[2010J01047

Determination of bisphenol A in environmental water samples by stir bar sorptive extraction based on molecularly imprinted polymer

以双酚A(bPA)为单体,利用整体材料“原位“聚合技术制备以分子印迹聚合物为涂层的吸附萃取搅拌棒(MIP-SbSE),然后与高效液相色谱(HPlC)-二极管阵列检测器联用,探讨其对环境水样bPA的选择萃取性能。优化萃取过程中吸附和解吸时间、解吸液种类以及基底PH值和离子强度对目标化合物的选择吸附性能。在最佳条件下,MIP-SbSE可对模板分子进行有效的选择吸附,线性范围为1.0~200μg/l,检出限(S/n=3)和定量限(S/n=10)分别为0.28μg/l和0.94μg/l。在实际水样分析中,具有良好的加标回收率,其值为96.0%~108.7%。研究结果表明,所建立的方法具有简便、灵敏和环境友好等特点。A new stir bar sorptive extraction (SBSE) based on molecularly imprinted polymer (MIP) with bisphenol A as template was prepared.Based on it,a simple,selective and sensitive method for the determination of bisphenol A (BPA) was developed combined with high performance liquid chromatography (HPLC) with diode array detection.To achieve the optimum extraction performance,several main parameters,including extraction and desorption time,the nature of desorption solvent,pH value and contents of inorganic salt in the sample matrix,were investigated.The optimized parameters for the extraction of BPA from water matrix with the MIP-SBSE are as follows: extraction and desorption time were 120 min and 10 min,respectively; the pH value of matrix was 10.0; using acetonitrile (including 1% acetic acid) as desorption solvent; no salt was added in the matrix.Under the optimized experimental conditions,the method showed good linearity between 1.0-200 μg/L.The detection limit (S/N=3) and quantification limit (S/N=10) of the proposed method for the BPA was 0.28 μg/L and 0.94 μg/L,respectively.The proposed method was successfully applied to the determination of the target compound in water samples.The recoveries of spiked target compound in real samples ranged from 96.0%-108.7%.The results indicated that the developed method possessed the advantages such as high sensitivity,simplicity,low cost and environmental friendliness.国家自然科学基金项目(No.20805039);福建省青年科技人才创新项目(No.2006F3117

Micro-extraction Determinationof Alkylphenolic Acids in Chinese Patent Medicine GBE with n-hexane Extract by LiquidChromatography - mass Spectrometry

正己烷萃取,并用HPLC-UV、HPLC-MS对中成药银杏浸膏(GBE)中微量烷基酚酸进行定性、定量分析。正己烷萃取效率高、共萃杂质少。在优化的实验条件下,平均回收率为98.9%(n=5)。银杏烷基酚酸(M=346)的HPLC-UV检测限为0.1μg/g,线性范围为0.5～10μg/g。With n-hexane extraction, the qualitative and quantitative analyses of alkylphenolic acids in Chinese patent medicineGBE (Ginkgo Bilobu Extract) were carried out with liquid chromatography-UV detector and mass spectrometry detector. Then-hexane was proven to be a very efficient extracting reagent, and few interfering materials were coextracted. Under the optimizedexperimental conditions, the recovery was 98.9%(n=5), the detection limit was 0.1μg/g, and the linear range was between 0.5～10μg/g for Ginkgo Biloba alkylphenolic acid of molecular weight of 346.厦门市科委夕阳红基金会资助项目(2000-1043

海水中痕量铜的双Sep-Pak柱FIA在线预富集和FAAS检测

采用配有双Sep-Pak柱的流动注射分析仪在线预富集海水样品中痕量铜的8-羟基喹啉络合物,经甲醇洗提后,由火焰原子吸收光谱仪检测,对100ml海水样品的富集倍率可达2个数量级,富集检测速率可为10次/h。多次富集测定的重现性在2.0～5.7％范围内,测定了铜含量在3～7ng/ml浓度范围内的海水样品

Preparation of sorbent based on porous monolith incorporated with graphene oxide nanosheets for stir cake sorptive extraction of strongly polar aromatic amines

National Natural Science Foundation of China [21377105, 21077085]; Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Ministry; New Century Excellent Talents in Fujian Province UniversityIn this study, poly(ethylene glycol dimethacrylate/graphene oxide) (EDMA/GO) monolith was prepared by one-step in situ polymerization. The porous monolith was used for the first time as the sorbent of stir cake sorptive extraction (SCSE) for the preconcentration of strongly polar aromatic amines (AAs) from water samples. The effect of the content of EDMA and GO in the monolith on the extraction efficiencies was investigated in detail. The sorbent was characterized by elemental analysis, transmission electron microscopy, scanning electron microscopy and infrared spectroscopy. Analysis of polar AAs in environmental water samples by a combination of poly(EDMA/GO)-SCSE and HPLC with diode-array detection was selected as a paradigm for the practical application of the new sorbent. Under the optimal conditions, the limits of detection (S/N = 3.0) of the developed method for AAs ranged from 0.04 to 0.19 mu g L-1. Good reproducibility of the method was obtained as intra-and inter-day precisions, the relative standard deviations (RSDs) were less than 4.0%. Finally, the proposed method was successfully applied to the determination of trace AAs in environmental water samples. The recoveries of AAs spiked in different matrices ranged from 74.2% to 105%, and RSDs of repeatability ranged from 1.6% to 9.6%