Evaluation of an analytical method for determining phthalate esters in wine samples by solid-phase extraction and gas chromatography coupled with ion-trap mass spectrometer detector
Evaluation of an analytical method for determining phthalate esters in wine samples by solid-phase extraction and gas chromatography coupled with ion-trap mass spectrometer detector
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DOI：
10.1007/s00216-011-5551-9
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发表时间：
2012-01-01
影响因子：
4.3
通讯作者：
Avino, Pasquale
中科院分区：
文献类型：
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作者：
Russo, Mario Vincenzo;Notardonato, Ivan;Avino, Pasquale
建立了固相萃取法（SPE），利用Carbograph - 1吸附剂对葡萄酒样品中6种邻苯二甲酸酯类物质进行萃取分析。固相萃取法对邻苯二甲酸酯（PAE）标准溶液的回收率为78% ~ 105%，相对标准偏差（RSD）为千分之一（6.5）；对PAE含量分别为20和50 ng mL（-1）的红酒样品的回收率为73 ~ 71% ~ 96 ~ 99%，相对标准偏差为千分之一（8.4）。报道了碳图1/水溶液的吸附等温线和突破曲线。采用气相色谱联用离子阱质谱仪（GC/IT-MS）进行分析。发现仪器分析方案在0.01-10.0 μ g mL（-1）范围内产生线性校准，R(2)值为千分之一日元0.9992。GC/IT-MS （SIM模式）的检测限在0.2至14 ng mL（-1）之间（RSD为千分之一货币符号5.6），而定量限在0.5至25 ng mL（-1）之间（RSD为千分之一货币符号5.9）；以RSD计算，葡萄酒样品的日内重复性和日内重复性分别在0.9-7.8和1.0-10.5之间。所建立的分析方法已应用于几种商品葡萄酒样品。此外，所研究的方法简单、可靠、可重复性好、成本低。
A solid-phase extraction (SPE) method was developed for extraction and analysis of six phthalate esters in wine samples using Carbograph 1 sorbent. The SPE procedure allowed efficient recovery of the investigated phthalates ranging between 78% and 105% with a relative standard deviation (RSD) a parts per thousand currency sign6.5 for an ethanolic phthalic acid ester (PAE) standard solution and between 73-71% and 96-99% with a RSD a parts per thousand currency sign8.4 for red wine samples spiked with 20 and 50 ng mL(-1) of PAE, respectively. The adsorption isotherms and breakthrough curves for Carbograph 1/water solution were reported. Gas chromatography coupled with an ion-trap mass spectrometer detector (GC/IT-MS) was used for analysis. The instrumental analytical protocol was found to yield a linear calibration in the range 0.01-10.0 mu g mL(-1) with R (2) values a parts per thousand yen0.9992. The limits of detection in GC/IT-MS (SIM mode) vary between 0.2 and 14 ng mL(-1) (RSD a parts per thousand currency sign5.6) whereas the limits of quantification range between 0.5 and 25 ng mL(-1) (RSD a parts per thousand currency sign5.9); the intra- and inter-day repeatabilities calculated as RSD for wine samples, were between 0.9-7.8 and 1.0-10.5, respectively. The analytical method developed was applied to several commercial wine samples. Furthermore, the investigated methods are simple, reliable, reproducible, and not expensive.