环境样品酞酸酯分析中溶剂背景的影响

选择环境样品酞酸酯分析中常用的有机溶剂,通过GC-MS对浓缩后的色谱纯、分析纯以及分析纯经过重蒸处理的有机溶剂进行11种酞酸酯背景测定。结果表明这些常用有机溶剂存在一定程度的酞酸酯污染,特别是邻苯二甲酸二正丁酯(DBP)和邻苯二甲酸二(2-乙基)己酯(DEHP)等2种环境样品中常见酞酸酯污染单体,最高浓度可达74.2μg/L(DBP)和64.3μg/L(DEHP)。有机溶剂用量大的酞酸酯分析方法(如土壤提取)需要对提取剂背景进行严格控制。     

气相色谱-质谱法同时测定动物内脏中的14种酞酸酯类环境激素残留

开展了动物内脏中14种酞酸酯类（PAEs）环境激素残留的气相色谱-电子轰击离子源/质谱（GC-EI/MS）的分析方法研究。优化与选择了动物内脏样品的前处理条件,动物内脏样品经正己烷/二氯甲烷（1/1,v/v）混合提取剂超声提取、Florisil硅藻土固相萃取柱净化与乙酸乙酯/正己烷（2/3,v/v）混合洗脱剂洗脱和浓缩后,以邻苯二甲酸二苯基酯（DPhP）为内标物,采用GC-EI/MS的选择离子监测方式（SIM）进行定性和定量分析。当猪肝样品的加标浓度水平为100、200、400 μg/kg时,加标回收率为：60%~110%,相对标准偏差为：0.78%~10.3%;除邻苯二甲酸二（2-甲氧基乙基）酯（DMEP）与邻苯二甲酸二（2-乙氧基乙基）酯（DEEP）的检测限（MDL）分别为3.30与2.25 μg/kg外,其余的12种PAEs的MDL ≦ 1.74 μg/kg;线性范围为50 ~ 800 μg/kg,相关系数都大于0.9994。此分析方法成功地应用于6种动物内脏中14种痕量PAEs残留的分析。     

GC-EI-MS内标法分析鱼肉中邻苯二甲酸酯

鱼肉样品以Florisil硅藻土层析柱净化后, 经气相色谱-电子轰击离子源-质谱法(GC-EI-MS)分析其中8种邻苯二甲酸酯(PAEs)含量: 邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丙酯(DPrP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二戊酯(DPeP)、邻苯二甲酸二环己基酯(DCHP)、邻苯二甲酸二己酯(DHP)、邻苯二甲酸二(2-乙基己基)酯(DEHP). 比较了外标和内标法定量, 并确定苯甲酸苄基酯为内标物; 优化了提取剂、吸附剂和洗脱剂的种类, 以及洗脱体积等样品前处理方法; 尤其对分析空白的控制问题进行了详细讨论; 准确分析了5种鱼样品中此类物质含量. 该方法的线性范围为50.0～800 μg•L^－1, 相关系数(R)大于0.99986, 相对标准偏差(Relative standard deviation, RSD)均小于12.7%, 检测限(Limit of detection, LOD)低于3.66 μg•L^－1, 样品的加标回收率为74.0%～113%. 其线性范围、相关系数、准确度、精密度和LOD等指标均满足鱼肉中多种PAEs同时分析的要求.     

固相萃取-反相高效液相色谱法测定水中的邻苯二甲酸酯

建立了固相萃取-反相高效液相色谱法检测水中3种邻苯二甲酸酯类物质邻苯二甲酸二甲酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二正辛酯的方法. 考察了固相萃取柱、洗脱溶剂、洗脱体积、上样速度以及洗脱速度对萃取效率的影响. 通过综合分析, 选定SupelcleanLC-18 SPE Tube固相萃取柱, 甲醇为洗脱剂, 洗脱体积2 mL, 上样速度为4 mL/min, 洗脱速度为1 mL/min. 在此萃取条件下, 萃取回收率在83.4%～121.2%之间. 邻苯二甲酸二甲酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二正辛酯质量浓度在2～100 mg/L之间均为线性. 经萃取后, 方法的最低检出限分别为邻苯二甲酸二甲酯0.06 μg/L, 邻苯二甲酸二(2-乙基己基)酯0.16 μg/L, 邻苯二甲酸二正辛酯0.08 μg/L. 方法的精密度在10%～15%之间. 应用该方法测定自来水中酞酸酯类化合物的含量, 加标回收率为83.6%～110.2%.     

快速提取-超高效液相色谱法测定唇膏中11种酞酸酯

建立快速提取–超高效液相色谱法测定唇膏中11种酞酸酯的检测方法。将唇膏样品涂覆在定量滤纸上,用甲醇涡旋超声提取,色谱柱采用Waters ACQUITY UPLC BEH C_(18)柱(100 mm×2.1 mm,1.7μm),流动相为乙腈–水,梯度洗脱,流量为0.5 mL/min,用PDA检测器检测,检测波长225 nm。以3倍空白噪音计,邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)的检出限分别为1,2 mg/kg;邻苯二甲酸二丙酯(DPRP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二戊酯(DPP)、邻苯二甲酸二己酯(DHXP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二(2–乙基)己酯(DEHP)、邻苯二甲酸二正辛酯(DNOP)的检出限为3 mg/kg;邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二异癸酯(DIDP)的检出限为30 mg/kg。方法的加标回收率为86.6%~98.6%,测定结果的相对标准偏差为0.6%~6.0%(n=6)。该方法样品处理简单,提取效率高,分离效果好且灵敏度高,结合色谱图和紫外光谱图,能快速准确测定唇膏中11种酞酸酯。     

固相萃取-气相色谱法测定纺织品中的邻苯二甲酸酯类环境激素

采用索氏提取法以正己烷为提取溶剂提取纺织品中的邻苯二甲酸酯类物质(PAEs),以强阴离子交换固相萃取(SPE)小柱净化本底杂质并富集待测物,建立了纺织品中10余种PAEs环境激素的同时测定方法。采用的固相萃取条件为:5 mL正己烷活化、3 mL异辛烷淋洗、2 mL含15%乙酸乙酯的正己烷溶液洗脱。SPE能有效地对提取液进行富集浓缩,同时对纺织物提取液中的杂质净化效果突出。该方法准确可靠,重现性好,在5~100 mg/kg 添加水平,PAEs各化合物的回收率为86.3%~102.7%,相对标准偏差（RSD）一般小于5%。检测的10余种PAEs中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丙酯(DPrP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二戊酯(DAP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二环己酯(DCHP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)、邻苯二甲酸二正辛酯(DNOP)的方法检出限小于1mg/kg,邻苯二甲酸二异壬酯(DINP)与邻苯二甲酸二异癸酯(DIDP）的方法检出限分别为1.74 mg/kg和1.55 mg/kg。     

毛细管气相色谱法测定化妆品中的酞酸酯

建立了用毛细管气相色谱配氢火焰离子化检测器测定化妆品中6种酞酸酯(邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二(2-乙基己)酯(DEHP)和邻苯二甲酸二正辛酯(DOP))的方法。样品用甲醇超声提取,经高速冷冻离心,清液经干燥脱水过0.5 μm滤膜过滤,直接注入气相色谱仪进行分析。然后,经过气相色谱-电子电离-质谱检测分析,确证气相色谱-氢火焰检测的阳性检出结果。用保留时间定性,外标法定量。6种酞酸酯的回收率为82.90%～     

气相色谱-电子轰击离子源质谱法分析卷烟和烟叶中29种农药的残留

开展了卷烟和烟叶中有机氯、有机磷和拟除虫菊酯3类29种农药残留的气相色谱-电子轰击离子源质谱(GC-EI/MS)的分析方法研究。优化与选择了卷烟和烟叶样品的前处理条件,样品经正己烷-丙酮(体积比为1∶1)混合提取剂超声提取、Florisil硅土和中性氧化铝双净化剂固相萃取柱净化、二氯甲烷-正己烷(体积比为95∶5)混合洗脱剂洗脱和浓缩后,以磷酸三苯酯(TPP)为内标物,采用GC-EI/MS的选择离子监测方式(SIM)进行定性和定量分析。当样品的加标水平为20,50,100 μg/kg时,加标回收率为70%～110%,相对标准偏差在2%～8%之间;除了甲氰菊酯、氯菊酯和溴氰菊酯的方法检出限(LOD)分别为1.85,1.74与2.54 μg/kg外,其余的26种农药的LOD均小于0.8 μg/kg;线性范围为5.0～500.0 μg/kg,相关系数都大于等于0.9994。此分析方法已成功地应用于卷烟和烟叶样品中3类29种痕量农药残留的分析     

牛奶中酞酸酯污染物的气相色谱质谱-联用测定

建立了气相色谱.质谱法(GC-MS)测定市售牛奶中4种酞酸酯(邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二异丁基酯(DiBP)、邻苯二甲酸二丁基酯(DBP),邻苯二甲酸二(2-乙基己基)酯(DEHP))的方法.样品采用乙酸乙酯直接萃取,C18小柱净化,过0.45μm滤膜,直接注入GC-Ms进行分析.保留时间定性,外标法定量.4种酞酸酯的回收率为77.9%～109.07%;精密度(RSD)为1.72%～6.18%;检测限在0.15～60 ng之间.     

基于PA6纳米纤维膜固相萃取-液相色谱法检测牛奶中的邻苯二甲酸酯

采用静电纺丝法制备了聚酰胺6(PA6)纳米纤维膜, 结合固相萃取技术-液相色谱法(HPLC-UV)检测了市售牛奶样品中的6种邻苯二甲酸酯(PAEs)的含量. 对影响实验的各种因素, 如提取溶剂的种类及用量、超声时间、洗脱溶剂的种类及用量、纳米纤维膜的用量、pH及过样速度等进行了考察. 在最优化条件下, 邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸丁基苄酯(BBP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-乙基己)酯(DEHP)和邻苯二甲酸二正辛酯(DOP)的检出限分别为0.02, 0.01, 0.05, 0.05, 0.10和0.25 ng/mL. 将该方法应用于不同品牌不同包装牛奶样品的检测, 只需2.5 mg PA6纳米纤维膜, 即可完全萃取样品中的PAEs, 相对标准偏差(RSD)小于5.82%, 回收率为93.40%~104.83%. 该方法测定牛奶中PAEs环境雌激素, 检出限低, 灵敏度高, 结果准确可靠, 重现性好.     

Preparation of polypyrrole-coated magnetic particles for micro solid-phase extraction of phthalates in water by gas chromatography-mass spectrometry analysis

In this work, polypyrrole (PPy)-coated Fe(3)O(4) magnetic microsphere were successfully synthesized, and applied as a magnetic sorbent to extract and concentrate phthalates from water samples. The PPy-coated Fe(3)O(4) magnetic microspheres had the advantages of large surface area, convenient and fast separation ability. The PPy coating of magnetic microspheres contributed to preconcentration of phthalates from water sample, due to the π-π bonding between PPy coating and the analytes. Also, the coating could prevent aggregation of the microspheres, and improve their dispersibility. In this study, seven kinds of phthalates were selected as model analytes, including dimethyl phthalate (DMP), diethyl phthalate (DEP), di-iso-butyl phthalate (DIBP), di-n-butyl phthalate (DBP), benzylbutyl phthalate (BBP), di-(2-ethylhexyl) phthalate (DEHP) and di-n-octyl phthalate (DNOP), and gas chromatography-mass spectrometry (GC-MS) was introduced to detect the phthalates after sample pretreatment. Important parameters of the extraction procedure were investigated, and optimized including eluting solvent, the amount of Fe(3)O(4)@PPy particles, and extraction time. After optimization, the procedure took only 15 min to extract and concentrate analytes with high efficiency. Validation experiments showed that the optimized method had good linearity (0.985-0.998), precision (3.4-11.7%), high recovery (91.1-113.4%), and the limits of detection were from 0.006 to 0.068 μg/L. The results indicated that the novel method had advantages of convenience, good sensitivity, high efficiency, and it could also be applied successfully to analyze phthalates in real water sample.     

薄层色谱扫描法测定塑料食品袋中酞酸酯的含量

建立了采用薄层色谱扫描测定塑料食品袋中4种酞酸酯(酞酸二甲酯(DMP)、酞酸二乙酯(DEP)、酞酸二丁酯(DBP)和酞酸二(2-乙基己基)酯(DEHP))的方法。经粉碎的样品先用乙醇浸泡24 h,然后超声提取,经0.45 μm滤膜过滤。点样在以丙酮处理过的硅胶G板上,以乙酸乙酯-无水乙醚-异辛烷(体积比为1∶4∶15)为展开剂展开,以双波长反射吸收飞点扫描测定(λS=275 nm,λR=340 nm),外标法定量。该法的线性关系较好,DMP、DEP、DBP和DEHP的检出限分别为2.1,2.4,3.4和4.0 ng,混合标准品在同一薄层板上的峰面积的相对标准偏差（RSD）为2.8%～3.5%,4种酞酸酯的样品加标回收率为78.58%～111.04%。该方法样品用量少,前处理简单,分离效果好,可用于塑料袋中4种酞酸酯的同时测定。经与气相色谱法的分析结果比较,两种方法对实际样品的分析结果接近。     

A novel quantitation method for phthalates in air using a combined thermal desorption/gas chromatography/mass spectrometry application

In this study, a novel quantitation method was developed to facilitate the simple and effective sampling and analysis of phthalates in air based on a sorbent tube-thermal desorption-gas chromatography-mass spectrometry system combination. The performance of the thermal desorption-based analysis was assessed using three different sorbent combinations [1]: quartz wool (QW) [2], glass wool (GW), and [3] quartz wool plus Tenax TA (QWTN) in terms of relative recovery in reference to a direct injection method. There was no significant difference in the average recovery rate for seven target phthalates based on sorbent tube type (QW, 70.2 ± 4.28; GW, 73.2 ± 8.8; and QWTN, 72.5 ± 5.02%). However, the recovery rate of phthalates in each sorbent tube type was distingusihed by physicochemical properties of the target compound (e.g., molecular weight and boiling point). The recovery rate of the QW tube was high for dimethyl phthalate and diethyl phthalate compared to other sorbent tubes, while that of the GW tube exhibited greater values for dibutyl phthalate, benzyl butyl phthalate, di(2-ethylhexyl) adipate, di(2-ethylhexyl) phthalate, and di-n-octyl phthalate. The simple sorbent tube-thermal desorption approach is feasible for the quantitation of seven phthalates present at 0.45–24.5 ng m⁻³ levels in actual air samples (20 L).     

Simultaneous screening and determination eight phthalates in plastic products for food use by sonication-assisted extraction/GC-MS methods

Studies on determination of eight kinds of phthalates, e.g. di-ethyl phthalate (DEP), di-propyl phthalate (DPP), di-isobutyl phthalate (DIBP), di-butyl phthalate (DBP), benzyl butyl phthalate (BBP), di-cyclohexyl phthalate (DCHP), di-(2-ethylhexyl) phthalate (DEHP), di-octyl phthalate (DOP), in 25 kinds of plastic products for food use, including packaging bags, packaging film, containers, boxes for microwave oven use, sucking tubes, spoons, cups, plates, etc. by gas chromatography in combination with mass spectrometry detector (GC-MS) in electronic ionisation mode (EI) with selected-ion monitoring (SIM) acquisition method (GC-MS (EI-SIM)) have been carried out. Methods have been developed for both qualitative and quantitative analysis of phthalates. Extraction, clean-up and analysis procedure have been optimized. Determination of samples were performed after frozen in liquid nitrogen and sonication-assisted extraction with hexane, clean-up with LC-C18 SPE and analyzed by GC-MS methods. The base peak (m/z = 149) of all the phthalates was selected for the screening studies. The characteristic ions, 121, 177, 222 for DEP; 191, 209 for DPP; 57, 223 for DIBP; 104 for DBP; 91, 132, 206 for BBP; 55, 167 for DCHP; 113, 167, 279 for DEHP; 279 for DOP were chosen for quantitative studies. These techniques are possible to detect phthalates at the level of 10.0 μg/kg. Overall recoveries were 82-106% with R.S.D. values at 3.8-10.2%. Only one of the 25 examined samples was free from phthalates. The rest 24 samples were found to contain at least three or more of these phthalates. The predominant phthalate detected in the studied samples was DEHP.     

污水中6种邻苯二甲酸酯的测定

采用同时蒸馏萃取法提取水样中的邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸丁基苄基酯、邻苯二甲酸二正辛酯、邻苯二甲酸二(2-乙基己基)酯6种邻苯二甲酸酯,用GC-MS进行定性和定量分析.对pH值、盐度和提取时间等影响因素进行优化.当pH值为2.0,NaCl加入量为5.0 g/L和提取时间为2.5 h时,目标化合物具有较好的回收率.优化条件下6种邻苯二甲酸酯的样品加标回收率为98%～105%,相对标准偏差为1.8%～5.6%,方法检出限为8.0～200.0 ng/L.方法成功应用于城市污水中该类化合物的监测.     

Determination of phthalates in milk and milk products by liquid chromatography/tandem mass spectrometry

A liquid chromatographic/tandem mass spectrometric method using pneumatically assisted electrospray ionisation (LC/ESI-MS/MS) was developed for determination of dibutyl phthalate (DBP), benzyl butyl phthalate (BBP), di-2-ethylhexyl phthalate (DEHP), di-'isononyl' phthalate (DINP) and di-'isodecyl' phthalate (DIDP) in milk and milk products including infant formulas. The phthalates were extracted by a mixture of tert-butyl methyl ether and hexane from liquid samples. DBP, BBP and DEHP were removed from fats by liquid/liquid extraction into acetonitrile while DINP and DIDP were cleaned up on deactivated silica. The phthalates were detected in positive ion mode after separation on a reversed-phase C5 analytical column. Two transition products were monitored for each compound. The detection limits related to the transition products of lowest abundance were in the range 5-9 microg/kg.     

Simple and rapid determination of phthalates using microextraction by packed sorbent and gas chromatography with mass spectrometry quantification in cold drink and cosmetic samples

A simple and rapid method using microextraction by packed sorbent coupled with gas chromatography and mass spectrometry has been developed for the analysis of five phthalates, namely, diethyl phthalate, benzyl‐n‐butyl phthalate, dicyclohexyl phthalate, di‐n‐butyl phthalate, and di‐n‐propyl phthalate, in cold drink and cosmetic samples. The various parameters that influence the microextraction by packed sorbent performance such as extraction cycle (extract–discard), type and amount of solvent, washing solvent, and pH have been studied. The optimal conditions of microextraction using C₁₈ as the packed sorbent were 15 extraction cycles with water as washing solvent and 3 × 10 μL of ethyl acetate as the eluting solvent. Chromatographic separation was also optimized for injection temperature, flow rate, ion source, interface temperature, column temperature gradient and mass spectrometry was evaluated using the scan and selected ion monitoring data acquisition mode. Satisfactory results were obtained in terms of linearity with R² >0.9992 within the established concentration range. The limit of detection was 0.003–0.015 ng/mL, and the limit of quantification was 0.009–0.049 ng/mL. The recoveries were in the range of 92.35–98.90% for cold drink, 88.23–169.20% for perfume, and 88.90–184.40% for cream. Analysis by microextraction by packed sorbent promises to be a rapid method for the determination of these phthalates in cold drink and cosmetic samples, reducing the amount of sample, solvent, time and cost.     

Simultaneous determination of seven phthalates and four parabens in cosmetic products using HPLC-DAD and GC-MS methods

Studies on the determination of seven kinds of phthalates, i.e. diethyl phthalate, dipropyl phthalate, dibutyl phthalate, benzyl butyl phthalate, dicyclohexyl phthalate, di-(2-ethylhexyl) phthalate, and dioctyl phthalate, and four parabens, i.e. methylparaben, ethylparaben, propylparaben, and butylparaben, in 15 kinds of cosmetic products, including hair sprays, perfumes, deodorants, cream, lotion, etc., by HPLC with diode array detection and GC-MS in electron impact ionization mode with selected-ion monitoring have been carried out. Methods have been developed for both qualitative and quantitative detection of phthalates and parabens. Extraction, clean-up, and analysis procedures have been optimized. HPLC and GC-MS determinations were performed after sonication-assisted extraction with methanol and clean-up with C18 SPE. These techniques permit detection of phthalates at a level of 10.0-100.0 microg/kg and of parabens at a level of 20.0-200.0 microg/kg. Overall recoveries were 85-108% with RSD values of 4.2-8.8%. Only one of the 15 examined samples was free from phthalates and parabens. The remaining 14 samples were found to contain at least three or more of these phthalates and/or parabens. The predominant phthalates and parabens detected in the studied samples were methylparaben, propylparaben, diethyl phthalate, dibutyl phthalate, dicyclohexyl phthalate, and di-(2-ethylhexyl) phthalate. The residue level is at 1.22-5289 mg/kg.     

Expanding the number of phthalates monitored in house dust

Phthalates have been used as plasticisers for several decades in various industry and consumer products. A method was developed for the determination of 13 not commonly monitored phthalates in household dust. The method was based on solvent extraction using sonication, sample clean-up by solid phase extraction (SPE), and analysis using isotope dilution gas chromatography-tandem mass spectrometry (GC/MS/MS). The method was applied to the analysis of dust samples collected using two vacuum sampling techniques from 38 urban Canadian homes: a sample of fresh or ‘active’ dust (FD) collected by technicians and a composite sample taken from the household vacuum cleaner (HD). Spearman rank correlations between HD and FD samples were significant for six phthalates with median concentrations above their method detection limits (MDLs), suggesting that the HD samples provide comparable results with FD samples. Seven phthalates were detected and quantified in a Canada-wide set of 126 household dust samples, among which six phthalates were detected at frequencies higher than 87%, with median (range) concentrations of 1.9 (<0.42–240) (μg/g) for diisohexyl phthalate (DIHxP), 3.8 (<0.16–260) (μg/g) for di-n-heptyl phthalate (DHepP), 6.6 (<1.1–1170) (μg/g) for diisooctyl phthalate (DIOP), 1.1 (<0.12–390) (μg/g) for di-n-octyl phthalate (DOP), 6.3 (<0.16–430) (μg/g) for dinonyl phthalate (DNP), and 1.8 (<0.18–850) (μg/g) for di-n-decyl phthalate (DDP). High detection frequencies and widely scattered concentration levels of these phthalates in this preliminary set of 126 samples suggested a high variability in potential exposure to phthalates in Canadian homes. NIST SRM 2585 (organic contaminants in house dust) was also analysed; eight phthalates were detected, with concentrations ranging from 6.0 μg/g for DOP to 79 μg/g for DIHxP. The results from SRM 2585 may contribute to the certification of phthalate concentration values in this SRM.     

Preparation and evaluation of molecularly imprinted solid-phase micro-extraction fibers for selective extraction of phthalates in an aqueous sample

A novel molecularly imprinted polymer (MIP) that was applied to a solid-phase micro-extraction (SPME) device, which could be coupled directly to gas chromatograph and mass spectrometer (GC/MS), was prepared using dibutyl phthalate (DBP) as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope images indicated that the MIP-coated solid-phase micro-extraction (MI-SPME) fibers were homogeneous and porous. The extraction yield of DBP with the MI-SPME fibers was higher than that of the non-imprinted polymer (NIP)-coated SPME (NI-SPME) fibers. The MI-SPME fibers had a higher selectivity to other phthalates that had similar structures as DBP. A method was developed for the determination of phthalates using MI-SPME fibers coupled with GC/MS. The extraction conditions were optimized. Detection limits for the phthalate samples were within the range of 2.17-20.84 ng L⁻¹. The method was applied to five kinds of phthalates dissolved in spiked aqueous samples and resulted in recoveries of up to 94.54-105.34%, respectively. Thus, the MI-SPME fibers are suitable for the extraction of trace phthalates in complicated samples.