A simple, environmentally friendly and high efficient extraction method was proposed for the determina- tion of five phthalates in aquatic products by gas chromatography combined with mass spectrometry detector （GC-M...A simple, environmentally friendly and high efficient extraction method was proposed for the determina- tion of five phthalates in aquatic products by gas chromatography combined with mass spectrometry detector （GC-MS）. When this method was adopted, samples were pretreated by modified QuEChERS（quick, easy, cheap, effective, rugged and safe） method. An environmentally friendly extractant（ethanol aqueous solution） replaced toxic acetonitrile for extracting phthalates in the protein-matrix samples. Fluorescence quenching spectra of bovine serum albumin（BSA） with phthalates show that there was a high-affinity interaction between phthalate and protein, de- creasing the extraction efficiency of phthalates from fish samples. However, in the 80%（volume fraction, ~） ethanol aqueous solution, a slow but full protein denaturation takes place, which would cause the unfolding of protein and the release of phthalates. Meanwhile, the fat-soluble impurities are extracted less in ^（ethanol） 80% aqueous solution than in either ~p（ethanol） 100% or hydrophobic solvents in the liquid-liquid extraction procedure. Therefore the puri- fication steps were greatly simplified. Overall recoveries were 81.77%--90.5% with limits of detection between 2.53 and 9.61 ~tg/L, and relative standard deviation values at 1.15%---4.85%. The proposed approach was satisfactorily applied to the determination of phthalates in real aquatic products, such as fish, shrimp and oyster.展开更多
Molecular fluorescence spectrometry, resonance Rayleigh scattering and gas chromatography-mass spectroscopy（GC-MS） were used to study the effect of pure fish serum albumin（FSA） as the model protein on the extracti...Molecular fluorescence spectrometry, resonance Rayleigh scattering and gas chromatography-mass spectroscopy（GC-MS） were used to study the effect of pure fish serum albumin（FSA） as the model protein on the extraction of three chlorobenzenes（CBs： 1,3-DCB, 1,2-DCB and 1,2,4-TCB; DCB=dichlorobenzene; TCB=trichlorobenzene） in fish samples. The results show that there was a strong binding effect between CB and FSA. In an aqueous solution of 90%（volume fraction） acetone, a slow but full protein denaturation might take place, which would cause the unfolding of protein and the releasing of CBs. Based on these results, a QuEChERS（quick, easy, cheap, effective, rugged and safe） method was modified by replacing the traditional acetonitrile with acetone aqueous solution in the present work. This modified QuEChERS method was applied in the determination of CBs in fish samples. The spiked recoveries and the limits of detection were 80.4%--118.3% and 2.4--7.3 ng/g, respectively. This paper proposes a new strategy by slowing down the protein denaturation and releasing bound organic compounds to enhance the extraction efficiency of CBs in fish samples.展开更多
采用串联固相萃取法(Extrelut-PRS-C18固相萃取柱萃取法、PRS-C18固相萃取柱萃取法)、MCX固相萃取柱萃取法和分散固相萃取法(QuEChERS(quick, easy, cheap, effective, rugged, and safe)法)4种前处理方法对肉制品中16种杂环胺(heterocy...采用串联固相萃取法(Extrelut-PRS-C18固相萃取柱萃取法、PRS-C18固相萃取柱萃取法)、MCX固相萃取柱萃取法和分散固相萃取法(QuEChERS(quick, easy, cheap, effective, rugged, and safe)法)4种前处理方法对肉制品中16种杂环胺(heterocyclic amines,HAs)进行提取,并从方法学和提取成本角度综合比较4种方法。结果表明:4种提取方法得到的16种HAs的回收率和精密度及检出限(limit of detection,LOD)和定量限(limit of quantification,LOQ)存在显著差异,其中QuEChERS法回收率和精密度均优于其他3种方法。MCX固相萃取柱萃取法和QuEChERS法的LOD和LOQ优于其他2种方法;MCX固相萃取柱萃取法和QuEChERS法所需经济和时间成本较低。综合分析,QuEChERS法具有快速、简便、便宜、有效、稳固和安全的特点,有利于肉制品中HAs的准确检测,并值得推广应用。展开更多
基金Supported by the National Natural Science Foundation of China（No.20973149） and the Natural Science Foundation of Shandong Province, China（No.ZR2011BM009）.
文摘A simple, environmentally friendly and high efficient extraction method was proposed for the determina- tion of five phthalates in aquatic products by gas chromatography combined with mass spectrometry detector （GC-MS）. When this method was adopted, samples were pretreated by modified QuEChERS（quick, easy, cheap, effective, rugged and safe） method. An environmentally friendly extractant（ethanol aqueous solution） replaced toxic acetonitrile for extracting phthalates in the protein-matrix samples. Fluorescence quenching spectra of bovine serum albumin（BSA） with phthalates show that there was a high-affinity interaction between phthalate and protein, de- creasing the extraction efficiency of phthalates from fish samples. However, in the 80%（volume fraction, ~） ethanol aqueous solution, a slow but full protein denaturation takes place, which would cause the unfolding of protein and the release of phthalates. Meanwhile, the fat-soluble impurities are extracted less in ^（ethanol） 80% aqueous solution than in either ~p（ethanol） 100% or hydrophobic solvents in the liquid-liquid extraction procedure. Therefore the puri- fication steps were greatly simplified. Overall recoveries were 81.77%--90.5% with limits of detection between 2.53 and 9.61 ~tg/L, and relative standard deviation values at 1.15%---4.85%. The proposed approach was satisfactorily applied to the determination of phthalates in real aquatic products, such as fish, shrimp and oyster.
基金Natural Science Foundation of Shandong Province,China
文摘Molecular fluorescence spectrometry, resonance Rayleigh scattering and gas chromatography-mass spectroscopy（GC-MS） were used to study the effect of pure fish serum albumin（FSA） as the model protein on the extraction of three chlorobenzenes（CBs： 1,3-DCB, 1,2-DCB and 1,2,4-TCB; DCB=dichlorobenzene; TCB=trichlorobenzene） in fish samples. The results show that there was a strong binding effect between CB and FSA. In an aqueous solution of 90%（volume fraction） acetone, a slow but full protein denaturation might take place, which would cause the unfolding of protein and the releasing of CBs. Based on these results, a QuEChERS（quick, easy, cheap, effective, rugged and safe） method was modified by replacing the traditional acetonitrile with acetone aqueous solution in the present work. This modified QuEChERS method was applied in the determination of CBs in fish samples. The spiked recoveries and the limits of detection were 80.4%--118.3% and 2.4--7.3 ng/g, respectively. This paper proposes a new strategy by slowing down the protein denaturation and releasing bound organic compounds to enhance the extraction efficiency of CBs in fish samples.
文摘采用串联固相萃取法(Extrelut-PRS-C18固相萃取柱萃取法、PRS-C18固相萃取柱萃取法)、MCX固相萃取柱萃取法和分散固相萃取法(QuEChERS(quick, easy, cheap, effective, rugged, and safe)法)4种前处理方法对肉制品中16种杂环胺(heterocyclic amines,HAs)进行提取,并从方法学和提取成本角度综合比较4种方法。结果表明:4种提取方法得到的16种HAs的回收率和精密度及检出限(limit of detection,LOD)和定量限(limit of quantification,LOQ)存在显著差异,其中QuEChERS法回收率和精密度均优于其他3种方法。MCX固相萃取柱萃取法和QuEChERS法的LOD和LOQ优于其他2种方法;MCX固相萃取柱萃取法和QuEChERS法所需经济和时间成本较低。综合分析,QuEChERS法具有快速、简便、便宜、有效、稳固和安全的特点,有利于肉制品中HAs的准确检测,并值得推广应用。
