Synthesis of [60]Fullerene-Fused Lactones via Carboxylic Acid Group-Directed C-H Bond Activation and Further Retro Baeyer-Villiger Reaction.

An efficient palladium-catalyzed reaction of [60]fullerene with benzoic acids via carboxylic acid group-directed C-H bond activation is achieved. The obtained [60]fullerene-fused lactones can undergo a retro Baeyer-Villiger reaction to provide [60]fullerene-fused ketones via apparent reduction in the presence of triflic acid. A representative ketone product obtained by the reduction reaction can be employed as an overcoating layer for the electron-transporting layer in an n-type perovskite solar cell.

[Determination of 118 pesticide residues in urine by ultra-high performance liquid chromatography-tandem mass spectrometry].

Pesticide residues in food and their hazardous effects have attracted much attention given the increased and widespread use of pesticides. The long-term consumption of food containing pesticide residues is an important pathway for the gradual accumulation of pesticides in the human body. Urine is often monitored as a biological sample for low-dose exposure to pesticides, and urine collection is a relatively convenient sampling technique in general population research.

Simultaneous Analysis of 53 Pesticides in Safflower ( L.) by Using LC-MS/MS Coupled with a Modified QuEChERS Technique.

Objective: An optimized quick, easy, cheap, effective, rugged, and safe (QuEChERS) technique was investigated and compared with the conventional QuEChERS technique for the simultaneous analysis of fifty-three pesticide residues in safflower using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS).

Method: Graphitic carbon nitride (g-CN) consisting of a major amount of carbon and nitrogen with a large surface area was used as a QuEChERS adsorbent instead of graphitized carbon black (GCB) for safflower extraction purification. Validation experiments were performed using spiked pesticide samples, and real samples were analyzed.

A new core-shell magnetic mesoporous surface molecularly imprinted composite and its application as an MSPE sorbent for determination of phthalate esters.

In this study, a new core-shell magnetic mesoporous surface molecularly imprinted polymer (FeO@SiO@mSiO-MIPs) which has specific adsorption and rapid adsorption rate for phthalate esters (PAEs) was prepared by a convenient method. Based on this composite as a magnetic solid phase extraction (MSPE) material, a rapid, efficient and sensitive matrix dispersion magnetic solid-phase extraction gas chromatography-mass spectrometry method (DMSPE-GC/MS) was developed for the determination of PAEs in multiple liquid samples. It is the first time that FeO@SiO@mSiO-MIPs have been prepared by bonding amino groups on the surface of a double layer silicon substrate with diisononyl phthalate (DINP) as virtual template and 3-(2-aminoethyl)-aminopropyl trimethoxymethylsilane (TSD) as functional monomer.

Retro Baeyer-Villiger reaction: thermal conversion of the [60]fullerene-fused lactones to ketones.

The conversion of the [60]fullerene-fused lactones to ketones with triflic anhydride as an unusual reductant under aerobic conditions has been achieved in excellent yields. The present thermal retro Baeyer-Villiger reaction from lactones to ketones has no precedents. In addition, the unique ring-opened peroxy [60]fullerene derivatives can be obtained by the electrochemical reactions of the synthesized [60]fullerene-fused ketones.

Magnetic solid-phase extraction based on sulfur-functionalized magnetic metal-organic frameworks for the determination of methylmercury and inorganic mercury in water and fish samples.

A novel magnetic metal-organic frameworks (FeO@UiO-66-SH) was successfully prepared by coating FeO nanospheres with sulfur-functionalized UiO-66. The FeO@UiO-66-SH possesses both the magnetic properties of FeO and the diverse properties of metal-organic framework (MOF) in one material, which has the superiority of high surface area, easy-operation and strong adsorb ability with mercury, is used for the magnetic solid-phase extraction of methylmercury (MeHg) and inorganic mercury (Hg) in water and fish samples. The analyzes were conducted by high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS).

Computational design and synthesis of molecular imprinted polymers for selective solid phase extraction of sulfonylurea herbicides.

A high-efficiency approach for the synthesis of molecularly imprinted polymers has been developed and further for the solid-phase extraction of sulfonylurea herbicides in food samples. Molecular simulation approach combined chemometric selected metsulfuron-methyl (MSM) and 2-trifluoromethyl acrylic acid (TFMAA) as the template and the monomer to synthesize the molecularly imprinted polymers (MIPs). Experimental validation confirmed that the MSM-imprinted polymers showed a higher selectivity and affinity to sulfonylurea herbicides.

Magnetic C nanospheres based solid-phase extraction coupled with isotope dilution gas chromatography-mass spectrometry method for the determination of sixteen polycyclic aromatic hydrocarbons in Chinese herbal medicines.

C-based magnetic nanospheres were synthesized by coating FeO nanospheres with silica, then modifying with 3-aminopropyltriethoxysilane as a linker and a C fullerene stationary phase. The morphologies, magnetic properties, infrared absorption and carbon content of magnetic nanospheres were studied by TEM, VSM, FTIR and carbon and sulfur analyzer. The magnetic nanospheres were employed for the magnetic solid-phase extraction (MSPE) of 16 polycyclic aromatic hydrocarbons (PAHs) in nine Chinese herbal medicines.

A retro Baeyer-Villiger reaction: electrochemical reduction of [60]fullerene-fused lactones to [60]fullerene-fused ketones.

A highly efficient electrochemical reduction of [60]fullerene-fused lactones to [60]fullerene-fused ketones, a formal process of retro Baeyer-Villiger reaction, has been achieved for the first time. The electrochemically generated dianionic [60]fullerene-fused lactones can be transformed into [60]fullerene-fused ketones in the presence of acetic acid in 85-91% yields. Control experiments have been performed to elucidate the reaction mechanism.

[Determination of 39 veterinary drug residues in Procambarusclarkii by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry].

An ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS) method was developed for determination of 39 veterinary drugs in Procambarusclarkii. Samples were extracted with acidified acetonitrile and purified with enhanced matrix removal-lipid (EMR-Lipid) adsorbent and graphitized multi-walled carbon nanotubes (GMWNTs). Extracts were analyzed by UHPLC-Q-TOF-MS.

Magnetic solid-phase extraction based on [60]fullerene functionalization of magnetic nanoparticles for the determination of sixteen polycyclic aromatic hydrocarbons in tea samples.

[60]Fullerene functionalized magnetic nanoparticles (FeO@SiO@C) were prepared and characterized by transmission electron microscope, vibrating sample magnetometer and infrared spectroscopy. The FeO@SiO@C was then applied for the magnetic solid-phase extraction of 16 priority pollutants polycyclic aromatic hydrocarbons (PAHs) in tea samples. The analyses were performed on gas chromatography-mass spectrometry (GC-MS) using selected ion monitoring (SIM) mode.

Synthesis of [60]Fullerene-Fused Spiroindanes by Palladium-Catalyzed Oxidative Annulation of [60]Fullerene with 2-Aryl Cyclic 1,3-Dicarbonyl Compounds.

A convenient and facile palladium-catalyzed reaction of [60]fullerene (C60) with 2-aryl cyclic 1,3-dicarbonyl compounds via the enolate-directed sp(2) C-H activation and sp(3) C-H functionalization has been exploited to synthesize the novel and rare C60-fused spiroindanes for the first time. This reaction is easy to perform with broad substrate scope and provides diversified products in 20-50% yields. A plausible reaction mechanism involving the palladium-catalyzed enolate-directed C-H activation and subsequent cyclization has been proposed, and the electrochemistry of the C60-fused spiroindanes has also been investigated.

Ferric Perchlorate Promoted Reaction of [60]Fullerene with N-Sulfonyl Aldimines: Synthesis and Functionalization of Fulleroxazolidines.

The rare fulleroxazolidines 2 were successfully synthesized by the facile ferric perchlorate promoted reaction of [60]fullerene with various N-sulfonyl aldimines 1. Further functionalization of fulleroxazolidines by arenes in the presence of boron trifluoride afforded 1,4-bisarylation products 4. A possible reaction mechanism for the formation of the fulleroxazolidines is proposed.

Palladium-catalyzed decarboxylative annulation of 2-arylbenzoic acids with [60]fullerene via C-H bond activation.

A convenient and highly efficient palladium-catalyzed decarboxylative annulation of 2-arylbenzoic acids with [60]fullerene has been exploited to synthesize the novel and scarce [60]fullerene-fused dihydrophenanthrenes. The use of Lewis acid ZnCl2 is crucial for the success of the present formal [4 + 2] annulation reaction. Plausible reaction pathways leading to the observed products have been proposed, and the electrochemistry of the fullerene products has also been investigated.