固相微萃取技术用于蔬菜及饮料中有害物质分析的应用研究
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摘要
固相微萃取(SPME)是九十年代发展起来的一种无溶剂萃取技术,它集采样、萃取、浓缩、进样于一体,具有简单、快速、高效、无污染、便携、易于与其它仪器联用等优点。近些年来,固相微萃取技术广泛应用于环境、食品和药物分析等领域。
本文采用自制的固相微萃取装置,用于食品基质中痕量有机污染物的分析；并改进了传统SPME装置,制备了纤维簇SPME装置,对其相关性能进行了评价。
以固相微萃取-气相色谱法建立了定量分析蔬菜中多环芳烃含量的方法。试验优化了温度、时间、盐浓度和搅拌速度等因素。最优条件：温度,60℃；时间,40min；NaCl浓度,60mg／g；搅拌速度,600r／m；pH值为5.0。在最优化萃取条件下,从线性范围、检测限、回收率和精密度四个方面进行了评价。方法的线性范围达3-4个数量级,相关系数大于0.9964,检测限为0.04-2.32ng／g,回收率为81.07-107.5%,相对标准偏差均小于11.6%。应用该方法检测了九种蔬菜中多环芳烃的含量,取得了较好的效果。
建立了以三苄基杯[6]芳烃为萃取头涂层的固相微萃取-气相色谱法测定非酒精饮料中酞酸酯的方法。采用L2556正交设计试验优化了萃取温度、时间、盐浓度和搅拌速度等因素。HS-SPME的最优化操作条件为：温度,100℃；时间,50分钟；NaCl浓度,180 g／L；搅拌速度,0 r／m。在最优条件下,该方法的线性范围达3-5个数量级,且相关系数大于0.995。由于三苄基杯[6]芳烃涂层对酞酸酯类化合物良好的选择性和高灵敏度,萃取在实际饮料基质中进行,检测限为0.015-0.298μg／L,回收率为87.9-108.3%,相对标准偏差为9.62-15.2%。应用此方法检测了12种饮料中的酞酸酯。
构建了一种装有3根探头(OH-TSO涂层)的新型固相微萃取装置。通过对苯系物、多环芳烃和酞酸酯类化合物的分析,证明了相对于传统的单根探头装置,在不延长萃取时间的前提下,该纤维簇探头装置具有更高的萃取效率。在相同的萃取条件下,对于苯系物,多根探头的萃取容量是单根探头的2.61-3.28倍；对于多环芳烃,为1.56-3.11倍；对于酞酸酯,则为2.19-7.14倍。而且,对于相同的分析对象,纤维簇探头得到的线性范围比单根探头的更宽,检测限也相对较低。
Solid-phase microextraction (SPME) was developed by Pawliszyn and co-workers in 1989. It successfully overcomes the inherent shortcomings of conventional sample preparation methods by integrating a number of sample handling operations such as extraction, preconcentration, and sample introduction for instrumental analysis into a single step. Within the past few years, it has been widely used for the pretreatment of complicated matrices in environmental, food and drug.
In this article, a series of applications in food were carried out by our lab-made SPME device. Moreover, we made some improvements at the basic of traditional SPME divice and evaluation its characteristics.
A headspace solid-phase microextraction (HS-SPME)/gas chromatographic technique for the quantitative analysis of polycyclic aromatic hydrocarbons was developed in this study. The extraction parameters such as extraction temperature, extraction time, salt concentration and stirring speed were optimized. The optimized extraction protocol was as follows:60℃of the extraction temperature,40 min of the extraction time, and 60 mg/g NaCl in concentration with agitation at 600 r/m, pH 5.0. Under the optimized conditions, a mini validation was performed and the following parameters were determined:limit of detection, precision, recovery and linearity. The linearity was very good in the considered concentration ranges (r>0.9964). Average recoveries ranged from 81.07% to 107.5% and showed good accuracy for the proposed analytical method. And relative standard deviation (RSD) for five replicate analyses was found to be less than 11.6%. The limit of detection (LOD) ranged from 0.04-2.32 ng/g for all compounds. The method was successfully applied for headspace analysis of nine vegetables samples.
A headspace solid-phase microextraction (HS-SPME), in conjunction with gas chromatography using a novel sol-gel calix[6]arene-contained fiber for the determination of phthalate acid esters (PAEs) in non-alcoholic beverages is described for the first time. A Taguchi's L25 (56) orthogonal array experimental design was introduced to optimize the extraction parameters such as extraction temperature, extraction time, salt concentration and stirring speed. The optimized conditions were as follows:100℃of the extraction temperature,50 min of the extraction time, and 180 g/L NaCl in concentration without agitation. Under the optimized conditions, the method showed linear response of three to five orders of magnitude with correlation coefficients (r) better than 0.995. Owing to the good selectivity and high sensitivity of this fiber to PAEs, the extraction was carried out in real beverage matrix and low detection limits of 0.015-0.298μg/L were achieved. The recoveries of standard addition tests amounted to 87.9%-108.3% and the relative standard deviation values varied from 9.62% to 15.2%. The method was applied to the analysis of 12 kinds of beverages and bis-2-ethylhexyl phthalate was the sole analyte detected in these samples.
An improved SPME device based on sol-gel hydroxy-terminated silicone oil (OH-TSO) coated multifibers (3 fibers) was constructed. The multifibers provided larger extracion capacity compared to a single fiber without increasing the extraction time. This result was explained by the analysis of benzene substitutes (BTEX), polycyclic aromatic hydrocarbons (PAHs) and phthalate acid esters (PAEs). Its extraction amount was 2.61-3.28 times larger than that by a single fiber for BTEX under the same conditions. For PAHs and PAEs, the multiplying factor was 1.56-3.11 and 2.19-7.41, respectively. The linearity obtained by the multifibers was much wider than that obtained by the single fiber and the limit of detection was much lower to each of the analytes.
本文采用自制的固相微萃取装置,用于食品基质中痕量有机污染物的分析；并改进了传统SPME装置,制备了纤维簇SPME装置,对其相关性能进行了评价。
以固相微萃取-气相色谱法建立了定量分析蔬菜中多环芳烃含量的方法。试验优化了温度、时间、盐浓度和搅拌速度等因素。最优条件：温度,60℃；时间,40min；NaCl浓度,60mg／g；搅拌速度,600r／m；pH值为5.0。在最优化萃取条件下,从线性范围、检测限、回收率和精密度四个方面进行了评价。方法的线性范围达3-4个数量级,相关系数大于0.9964,检测限为0.04-2.32ng／g,回收率为81.07-107.5%,相对标准偏差均小于11.6%。应用该方法检测了九种蔬菜中多环芳烃的含量,取得了较好的效果。
建立了以三苄基杯[6]芳烃为萃取头涂层的固相微萃取-气相色谱法测定非酒精饮料中酞酸酯的方法。采用L2556正交设计试验优化了萃取温度、时间、盐浓度和搅拌速度等因素。HS-SPME的最优化操作条件为：温度,100℃；时间,50分钟；NaCl浓度,180 g／L；搅拌速度,0 r／m。在最优条件下,该方法的线性范围达3-5个数量级,且相关系数大于0.995。由于三苄基杯[6]芳烃涂层对酞酸酯类化合物良好的选择性和高灵敏度,萃取在实际饮料基质中进行,检测限为0.015-0.298μg／L,回收率为87.9-108.3%,相对标准偏差为9.62-15.2%。应用此方法检测了12种饮料中的酞酸酯。
构建了一种装有3根探头(OH-TSO涂层)的新型固相微萃取装置。通过对苯系物、多环芳烃和酞酸酯类化合物的分析,证明了相对于传统的单根探头装置,在不延长萃取时间的前提下,该纤维簇探头装置具有更高的萃取效率。在相同的萃取条件下,对于苯系物,多根探头的萃取容量是单根探头的2.61-3.28倍；对于多环芳烃,为1.56-3.11倍；对于酞酸酯,则为2.19-7.14倍。而且,对于相同的分析对象,纤维簇探头得到的线性范围比单根探头的更宽,检测限也相对较低。
Solid-phase microextraction (SPME) was developed by Pawliszyn and co-workers in 1989. It successfully overcomes the inherent shortcomings of conventional sample preparation methods by integrating a number of sample handling operations such as extraction, preconcentration, and sample introduction for instrumental analysis into a single step. Within the past few years, it has been widely used for the pretreatment of complicated matrices in environmental, food and drug.
In this article, a series of applications in food were carried out by our lab-made SPME device. Moreover, we made some improvements at the basic of traditional SPME divice and evaluation its characteristics.
A headspace solid-phase microextraction (HS-SPME)/gas chromatographic technique for the quantitative analysis of polycyclic aromatic hydrocarbons was developed in this study. The extraction parameters such as extraction temperature, extraction time, salt concentration and stirring speed were optimized. The optimized extraction protocol was as follows:60℃of the extraction temperature,40 min of the extraction time, and 60 mg/g NaCl in concentration with agitation at 600 r/m, pH 5.0. Under the optimized conditions, a mini validation was performed and the following parameters were determined:limit of detection, precision, recovery and linearity. The linearity was very good in the considered concentration ranges (r>0.9964). Average recoveries ranged from 81.07% to 107.5% and showed good accuracy for the proposed analytical method. And relative standard deviation (RSD) for five replicate analyses was found to be less than 11.6%. The limit of detection (LOD) ranged from 0.04-2.32 ng/g for all compounds. The method was successfully applied for headspace analysis of nine vegetables samples.
A headspace solid-phase microextraction (HS-SPME), in conjunction with gas chromatography using a novel sol-gel calix[6]arene-contained fiber for the determination of phthalate acid esters (PAEs) in non-alcoholic beverages is described for the first time. A Taguchi's L25 (56) orthogonal array experimental design was introduced to optimize the extraction parameters such as extraction temperature, extraction time, salt concentration and stirring speed. The optimized conditions were as follows:100℃of the extraction temperature,50 min of the extraction time, and 180 g/L NaCl in concentration without agitation. Under the optimized conditions, the method showed linear response of three to five orders of magnitude with correlation coefficients (r) better than 0.995. Owing to the good selectivity and high sensitivity of this fiber to PAEs, the extraction was carried out in real beverage matrix and low detection limits of 0.015-0.298μg/L were achieved. The recoveries of standard addition tests amounted to 87.9%-108.3% and the relative standard deviation values varied from 9.62% to 15.2%. The method was applied to the analysis of 12 kinds of beverages and bis-2-ethylhexyl phthalate was the sole analyte detected in these samples.
An improved SPME device based on sol-gel hydroxy-terminated silicone oil (OH-TSO) coated multifibers (3 fibers) was constructed. The multifibers provided larger extracion capacity compared to a single fiber without increasing the extraction time. This result was explained by the analysis of benzene substitutes (BTEX), polycyclic aromatic hydrocarbons (PAHs) and phthalate acid esters (PAEs). Its extraction amount was 2.61-3.28 times larger than that by a single fiber for BTEX under the same conditions. For PAHs and PAEs, the multiplying factor was 1.56-3.11 and 2.19-7.41, respectively. The linearity obtained by the multifibers was much wider than that obtained by the single fiber and the limit of detection was much lower to each of the analytes.
引文
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