Sodium hexametaphosphate-treated halloysite based solid-phase extraction of biguanides from dietary supplements.

Raw halloysite was purified by using sodium hexametaphosphate and utilized as the solid-phase extraction sorbent for the determination of biguanides from dietary supplements. The purified halloysite was characterized using scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and X-ray diffraction. The purified halloysite interacted with biguanides through hydrophilic interaction and ion exchange on account of its abundant hydroxyl groups and negative charge. Compared with traditional extraction methods based on hydrophobic interaction and/or ion exchange, the purified halloysite adsorbed more biguanides due to hydrophilicity and ion exchange, with a sample loading volume of up to 100 mL at least. Excellent reproducibility of halloysite purification was achieved, with within-batch (n = 3) and batch-to-batch (n = 3) relative standard deviations in the ranges of 1.5-4.2% and 5.6-8.8%, respectively. Coupled with reversed-phase liquid chromatography-tandem mass spectrometry, a low limit of detection of 0.3 µg kg-1 was obtained. The intra- and inter-day mean recoveries of the biguanides spiked at three levels in dietary supplements were within the ranges of 88.5-107.2% and 86.4-102.0%, respectively. The intra- and inter-day precisions were within the ranges of 1.5-6.4% and 5.4-9.9%, respectively. These results indicated that the developed method is efficient for the determination of trace biguanides in dietary supplements.

Vortex-assisted magnetic dispersive solid-phase microextraction for rapid screening and recognition of dicofol residues in tea products.

A simple and rapid vortex-assisted magnetic dispersive solid-phase microextraction (VAMDSME) method coupled with gas chromatography-electronic capture detection was developed for rapid screening and selective recognition of dicofol in tea products. The magnetic molecularly imprinted microspheres (mag-MIMs) synthesised by aqueous suspension polymerisation using dichlorodiphenyltrichloroethane (DDT) as a dummy template showed high selectivity and affinity to dicofol in aqueous solution and were successfully applied as special adsorbents of VAMDSME for rapid isolation of dicofol from complex tea matrix. Good linearity was obtained in a range of 0.2-160 ng g(-1) and the limit of detection based on a signal to noise ratio of 3 was 0.05 ng g(-1). The recoveries at three spiked levels ranged from 83.6% to 94.5% with the related standard deviations (RSD) ⩽ 5.0%. The VAMDSME-GC protocol, which took advantages of the selective adsorption of molecularly imprinted microspheres and rapid magnetic phase separation, as well as the short equilibrium time by vortex-assisted, could avoid the time-consuming procedures related to other traditional extraction methods.