A multifunctional magnetic graphene surface-enhanced Raman scattering (SERS) substrate was fabricated successfully by the layer-by-layer assembly of silver and graphene oxide (GO) nanoparticles (NPs) on the magnetic ferroferric oxide particles (Fe3O4@GO@Ag). This ternary particle possesses magnetic properties, SERS activity, and adsorption ability simultaneously. Owing to the multifunction of this Fe3O4@GO@Ag ternary complex, we put forward a new method called a surface magnetic solid-phase extraction (SMSPE) technique, for the SERS detections of pesticide residues on the fruit peels. SMSPE integrates many sample pretreatment procedures, such as surface extraction, separation sample, and detection, all-in-one. So this method shows great superiority in simplicity, rapidity, and high efficiency above other standard methods. The whole detection process can be finished within 20 min including the sample pretreatment and SERS detection. Owing to the high density of Ag NPs, the detection sensitivity is high enough that the lowest detectable concentrations are 0.48 and 40 ng/cm(2) for thiram and thiabendazole, which are much lower than the maximal residue limits in fruit prescribed by the U.S. Environmental Protection Agency. This multifunctional ternary particle and its corresponding analytical method have been proven to be applicable for practical samples and also valuable for other surface analysis.
The members of the Old Yellow Enzyme (OYE) family are capable of catalyzing the asymmetric reduction of (E/Z)-citral to (R)-citronellal—a key intermediate in the synthesis of L-menthol. The applications of OYE-mediated biotransformation are usually hampered by its insufficient enantioselectivity and low activity. Here, the (R)-enantioselectivity of Old Yellow Enzyme from Saccharomyces cerevisiae CICC1060 (OYE2y) was enhanced through protein engineering. The single mutations of OYE2y revealed that the sites R330 and P76 could act as the enantioselectivity switch of OYE2y. Site-saturation mutagenesis was conducted to generate all possible replacements for the sites R330 and P76, yielding 17 and five variants with improved (R)-enantioselectivity in the (E/Z)-citral reduction, respectively. Among them, the variants R330H and P76C partly reversed the neral derived enantioselectivity from 32.66% e.e. (S) to 71.92% e.e. (R) and 37.50% e.e. (R), respectively. The docking analysis of OYE2y and its variants revealed that the substitutions R330H and P76C enabled neral to bind with a flipped orientation in the active site and thus reverse the enantioselectivity. Remarkably, the double substitutions of R330H/P76M, P76G/R330H, or P76S/R330H further improved (R)-enantioselectivity to >99% e.e. in the reduction of (E)-citral or (E/Z)-citral. The results demonstrated that it was feasible to alter the enantioselectivity of OYEs through engineering key residue distant from active sites, e.g., R330 in OYE2y.
Molecularly imprinted polymers (MIPs) have the ability of predesigned specific recognition that can be selected to construct reliable functional materials. Combining the MIPs with magnetic nanoparticles results in magnetic MIPs (MMIPs) which possess both facile manipulation and high selectivity. In this report, MMIP microspheres are fabricated by coating a layer of MIPs on Fe3O4@Ag for SERS-based sensing of molecular species. The obtained Fe3O4@Ag@MIPs are further applied for simple, rapid, ultrasensitive, and label-free SERS detection of sibutramine (SIB, illegal additive), with a low LOD of 1.0 × 10–9 M. Moreover, the MMIP microspheres exhibit ultrahigh adsorption efficiency, selectivity, reusability, and good structural stability, which demonstrates the potential application for SERS. Particularly, the proposed approach of MMIPs-SERS can be successfully applied to quick screening of SIB in slimming supplements such as capsules, tea powder, and tablets, and the content for those is 6.18, 13.61, and 3.09 mg g–1, respectively. These properties make MMIP microspheres a promising SERS substrate to detect illegal additives in health-related products and chemical pollutants in the environment.
Discrimination of illegal cooking oil is a conundrum in the fields of analytical chemistry and food safety due to complicated sample systems, lack of common targets, and stringent demand of ultrahigh detection sensitivity for corresponding analytical methods. Capsaicin, one of the exogenous molecules that is subsistent in recycled kitchen waste oils, can be regarded as a target for illegal cooking oil identification. Nowadays, tracing capsaicin in oils is implemented mainly by high-performance liquid chromatography–mass spectrometry, which displays shortcomings in high costs and incapableness for field test. Here, we established a surface-enhanced resonance Raman scattering approach to detect capsaicin and identify illegal cooking oils by means of the molecular derivatization treatment of capsaicin. This method features high detection sensitivity with the detection limit of 1.0 × 10 –8 M, rapid response (<7 min detection duration), and simplicity in sample pretreatment, which is available for fast field test of illegal cooking oils.
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