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In this work, a novel method of TiO2 nanoparticles (NPs) functionalized monolithic capillary microextraction (CME) online coupling with inductively coupled plasma mass spectrometry (ICPMS) was developed for the sequential determination of Gd(3+) and Gd-based contrast agents in human urine samples. The monolithic capillary was prepared by embedding anatase TiO2 NPS in the poly(methacrylic acid-ethylene glycol dimethacrylate) (MAA-EDMA) framework. The Gd(3+) and Gd-based contrast agents (such as gadolinium-diethylene triamine pentaacetic acid (Gd-DTPA) and Gd-DTPA-bismethylamide (Gd-DTPA-BMA)) display different adsorption behaviors on the prepared monolithic capillary which possesses the adsorption properties of both anatase TiO2 NPS and poly(MAA-EDMA) monolith. Under the optimized conditions, the limits of detection (LODs) were found to be 3.6, 3.2, and 4.5 ng L(-1) for Gd(3+), Gd-DTPA, and Gd-DTPA-BMA, respectively, which are the lowest up to date. The enrichment factor was 25-fold with the sample throughput of 5 h(-1). The proposed method was validated by the analysis of Gd(3+) and Gd-DTPA in the healthy human urine samples as well as Gd(3+) and Gd-DTPA-BMA in patient urine samples. It was found that only a small amount of the free Gd(3+) was released from Gd-DTPA-BMA, and accurate results could be obtained since no oxidation/reduction or subtraction is involved in this method. This method is simple, sensitive, and rapid and provides a very attractive nonchromatography strategy for the speciation of Gd(3+) and Gd-based contrast agents in urine samples.

The pursuit of high-throughput sample analysis from complex matrix demands development of multiple ionization techniques with complementary specialties. A versatile integrated ambient ionization source (iAmIS) platform is proposed in this work, based on the idea of integrating multiple functions, enhancing the efficiency of current ionization techniques, extending the applications, and decreasing the cost of the instrument. The design of the iAmIS platform combines flowing atmospheric pressure afterglow (FAPA) source/direct analysis in real time (DART), dielectric barrier discharge ionization (DBDI)/low-temperature plasma (LTP), desorption electrospray ionization (DESI), and laser desorption (LD) technique. All individual and combined ionization modes can be easily attained by modulating parameters. In particular, the FAPA/DART&DESI mode can realize the detection of polar and nonpolar compounds at the same time with two different ionization mechanisms: proton transfer and charge transfer. The introduction of LD contributes to the mass spectrometry imaging and the surface-assisted laser desorption (SALDI) under ambient condition. Compared with other individual or multi-mode ion source, the iAmIS platform provides the flexibility of choosing different ionization modes, broadens the scope of the analyte detection, and facilitates the analysis of complex samples. Graphical abstract ᅟ.

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Supercritical fluid chromatography (SFC), which uses supercritical fluid with higher diffusivity and lower viscosity than liquid as its mobile phase, can provide fast, green, high-throughput and good performance methods for the analysis of complicated samples. It is an advantageous alternative for the separation of polar and nonpolar compounds, and even chiral isomers. As an important constituent of living organisms, lipids and the related lipidomics researches have attracted dramatic attention during the past years. The separation and identification of lipids and lipid isomers are of great significance and remain challenging. In this mini-review, the principle of SFC and its applications in lipid isomer separation are summarized.

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A new model-based sensor fault diagnosis (FD) scheme, using an equivalent model, is developed for a kind of Multiple Inputs Multiple Outputs (MIMO) nonlinear system which fulfills the Lipschitz condition. The equivalent model, which is a bank of one-dimensional linear state equations with the bounded model uncertainty, can take the place of a plant's exact nonlinear model in the case of sensor FD. This scheme shows a new perspective whereby, by using the equivalent model, it doesn't have to study the nonlinear internal structure character or get the exact model. The influence of the model uncertainty on the residuals is explained in this paper. A method, called pretreatment, is utilized to minimize the model uncertainty. The eigenstructure assignment method with assistant state is employed to solve the problem of perfect decoupling against the model uncertainty, disturbance, system faults, the relevant actuator faults, or even the case of no input from the relevant actuator. The realization of the proposed scheme is given by an algorithm according to a single sensor FD, and verified by a simulation example. Depending on the above, a sensor fault monitoring system is established by the sensor network and diagnosis logic, then the effectiveness is testified by a simulation.