[Determination of 18 polycyclic aromatic hydrocarbons in plastic products by ultra performance convergence chromatography].

A method for rapid determination of naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo (a) anthracene, chrysene, benzo(b) fluoranthene, benzo(k) fluoranthene, benzo(j) fluoranthene, benzo (e) pyrene, benzo (a) pyrene, indeno (1, 2, 3-cd) pyrene, dibenzo (a, h) anthracene, benzo (g, h, i) perylene in plastic products by ultra performance convergence chromatography (UPC2) coupled photodiode array detector (PAD) was developed. The 18 polycyclic aromatic hydrocarbons (PAHs) were successfully separated in less than 8.5 min on a Daicel IB-3 chiral column with a mobile phase of CO2, the mobile-phase additive of methanol/acetonitrile (25 :75, v/v) at column temperature of 40 degrees C, and a back pressure of 15.17 MPa. There was a linear correlation between peak area and PAH concentration in the range of 0.05-50 mg/L (r ≥ 0.999 5) for each PAH. The limits of quantification (LOQs)(S/N > 10) were 0.05 mg/L. After ultrasonic-assisted extraction in toluene, the sample was analyzed by UPC2-PDA. The recoveries of PAHs spiked in plastic samples were from 78.3% to 117.6%, and the repeatabilities of peak areas for the 18 PAHs were less than 5% (RSD, n = 5). The present UPC2-PDA method has the advantages of rapid speed, high resolution, and low organic reagent consumption.

[Determination of five coumarins in toys by high performance liquid chromatography-tandem mass spectrometry].

A rapid analytical method for the determination of five coumarins (coumarin, 7-methoxycoumarin, dihydrocoumarin, 7-methyl coumarin and 7-ethoxy-4-methyl coumarin) in toys by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been developed. After ultrasonic extraction in tetrahydrofuran, the samples were analyzed by HPLC-MS/MS in multi-reaction monitoring (MRM) mode. Acetonitrile and 0.1% acetic acid were used as the mobile phases with gradient elution. The linear ranges of calibration curves were 10 - 1 000 microg/L, and the limits of quantification (LOQ) (S/N > 10) were 2.0 microg/L for all the analytes, except that the LOQ for dihydrocoumarin was 5.0 microg/L. The recoveries of the five coumarins spiked in three types of samples were in the ranges of 93.2% - 105.8%, 97.3% - 103.2% and 96.8% - 102.9%, with the relative standard deviations in the ranges of 4.35% - 8.27%, 3.65% - 6.73% and 4.03% - 6.45%, respectively. The method was applied in the determination of 12 toy samples. The five analytes were found in 9 samples, and in some cases, the presence of quite high concentrations of these coumarins in the toys should be a matter of concern.

[Determination of 3 isothiazolinone preservatives in toys using liquid chromatography-tandem mass spectrometry].

A rapid analytical method for the determination of 3 isothiazolinone preservatives (2-methyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one and 1,2-benzylisothiazolin-3-one) in toys using liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed. After ultrasonic extraction with water, the analytes in the sample were separated and analyzed by LC-MS/MS under the isocratic elution of methanol and water (15:85, v/v) and in selected-reaction monitoring (SRM) mode. The linear ranges of calibration curves for the 3 analytes were 2.0 - 1 000 microg/L. The limit of quantification was 0.04 mg/kg for all the 3 analytes, which was lower than that of the method recommended by the European Toy Safety Directive in EN71-11-2005. The recoveries of the spiked standards in the two toy samples were 95.9% - 105.2% and 94.7% - 102.8% with the relative standard deviation ranges from 3.04% to 4.96% and from 2.36% to 4.79%, respectively. The method was applied in the determination of 10 toy samples, and the results can meet the requirements of the European Toy Safety Directive in EN71-9-2005 for the determination of isothiazolinones in toys.

Preparation of magnetic core mesoporous shell microspheres with C18-modified interior pore-walls for fast extraction and analysis of phthalates in water samples.

In this study, core-shell magnetic mesoporous microspheres with C18-functionalized interior pore-walls were synthesized through coating Fe(3)O(4) microspheres with a mesoporous inorganic-organic hybrid layer with a n-octadecyltriethoxysilane (C18TES) and tetraethyl orthosilicate (TEOS) as the silica source and cetyltrimethylammonia bromide (CTAB) as a template. The obtained C18-functionalized Fe(3)O(4)@mSiO(2) microspheres possess numerous C18 groups anchored in the interior pore-walls, large surface area (274.7 m(2)/g, high magnetization (40.8 emu/g) and superparamagnetism, uniform mesopores (4.1 nm), which makes them ideal absorbents for simple, fast, and efficient extraction and enrichment of hydrophobic organic compounds in water samples. Several kinds of phthalates were used as the model hydrophobic organic compounds to systematically evaluate the performance of the C18-functionalized Fe(3)O(4)@mSiO(2) microspheres in extracting hydrophobic molecules by using a gas chromatography-mass spectrometry. Various parameters, including eluting solvent, the amounts of absorbents, extraction time and elution time were optimized. Hydrophobic extraction was performed in the interior pore of magnetic mesoporous microspheres, and the materials had the anti-interference ability to macromolecular proteins, which was also investigated in the work. Under the optimized conditions, C18-functionalized Fe(3)O(4)@mSiO(2) microspheres were successfully used to analyze the real water samples. The results indicated that this novel method was fast, convenient and efficient for the target compounds and could avoid being interfered by macromolecules.

Preparation of Fe3O4@C@PANI magnetic microspheres for the extraction and analysis of phenolic compounds in water samples by gas chromatography-mass spectrometry.

In this work, core-shell structure Fe(3)O(4)@C@polyaniline magnetic microspheres were synthesized using simple hydrothermal reactions. The carbon-coated magnetic microspheres (Fe(3)O(4)@C) were first synthesized by a hydrothermal reaction, and then aniline was polymerized on the magnetic core via another hydrothermal reaction. Then, the obtained Fe(3)O(4)@C@polyaniline magnetic microspheres were applied as magnetic adsorbents for the extraction of aromatic molecules due to π-π interactions between polyaniline shell and aromatic compounds. In our study, five kinds of phenols including phenol, 2,4-dichlorophenol (DCP), 2,4,5-trichlorophenol (TCP), pentachlorophenol (PCP) and bisphenol A (BPA) were selected as the model analytes to verify the extraction ability of Fe(3)O(4)@C@PANI microspheres. After derivatization, the phenols were detected using gas chromatography-mass spectrometry (GC-MS). The dominant parameters affecting enrichment efficiency were investigated and optimized. Under the optimal conditions, the proposed method was evaluated, and applied to the analysis of phenols in real water samples. The results demonstrated that our proposed method based on Fe(3)O(4)@C@polyaniline magnetic microspheres had good linearity (r(2)>0.991), and limits of quantification (2.52-29.7 ng/mL), high repeatability (RSD<13.1%) and good recovery (85.3-110.6%).

Determination of iodine and bromine in coal and atmospheric particles by inductively coupled plasma mass spectrometry.

Bromine and iodine in atmospheric particles or coal can cause environmental problems such as destruction of ozone in the atmosphere; therefore, the presence of these compounds has recently received increased attention. Here, a rapid and reliable method for the simultaneous determination of total bromine and iodine using ICP-MS analysis is described. Samples were dissolved in mixtures of 5 mL of HNO(3) and 2 mL of H(2)O(2) in a high pressure microwave digester. The solution was then oxidized by per-sulfate (Na(2)S(2)O(8)) in addition to a small amount of silver nitrate, after which the total bromine and iodine were measured simultaneously by ICP-MS. The signal memory effects of bromine and iodine during analysis were effectively decreased by washing with a new mixture agent (2% alcohol acidic solution, pH 1-2 adjusted with HCl). The detection limits for bromine and iodine using this method were about 3.2 microg L(-1) and 1.1 microg L(-1), respectively. Additionally, the spike recoveries were between 78.7% and 121% for bromine and iodine analysis, while the relative standard deviations ranged from 4.3% to 9.7%, and from 1.5% to 3.4% for bromine and iodine, respectively. The results of this study indicate that the method described here is suitable for the analysis of micro-amounts of bromine and iodine in atmospheric particles and coal samples.