Development of an online µ-matrix cartridge extraction method for fipronil extraction in contaminated soils.

Nowadays, environment fate and behavior of pesticides in soil is still not fully understood due to the lack of standardized soil extraction method. In this work, a soil-filled micro-matrix cartridge was online combined with high performance liquid chromatography-mass spectrometry (HPLC-MS) through a six-way valve for the simultaneous extraction and determination of residual fipronil in soil. Compared with conventional extraction methods, such as hydroxypropyl-ß-cyclodextrin (HPCD) extraction, shaking extraction, ultrasonic-assisted extraction (UAE), three-step extraction and matrix solid phase dispersion (MSPD), the novel, miniaturized, and integrated online micro-matrix cartridge extraction (online µ-MCE) method exhibited better performance in terms of desorption efficiency (99.4%), analysis time, solvent consumption, sensitivity, and automation. In sequential extraction, online µ-MCE could further desorb fipronil from the extracted soil with the percentage of 1.05%-58.55%. High recovery of 92.69% obtained for the ISO certificated test-soil verified the satisfactory accuracy of the method. Besides, its wide universality was also validated in three variables: 1) various pesticides-soil interactions, 2) four types of compounds (aromatic hydrocarbons, carboxylic acids, alcohols and aldehydes), and 3) three types of soils (sandy soil, silty loam and silty clay). The superior desorption capacity might be attributed to the instantaneously increased high-pressure, continuous flow dynamic desorption and short residence time. The present encouraging findings might shed light on new ways to develop a mild, highly efficient, reliable and one-fit-all extraction method toward pesticide contaminated soil.

Study on the environmental fate of three insecticides in garlic by in vivo sampling rate calibrated-solid phase microextraction-gas chromatography-mass spectrometry.

Traditional sample preparation methods for insecticide analysis are laborious and fatal to living organisms. In the work, an in vivo sampling rate calibrated-solid phase microextraction-gas chromatography-mass spectrometry method was established and successfully used for in vivo sampling and quantitative determination of three insecticides (hexachlorobenzene, fipronil and chlorfenapyr) by direct exposing micron-sized fiber in living garlic. Absorption, enrichment, migration and elimination behavior of insecticides in garlic were investigated. Bioaccumulative effects with obvious tissue differences were observed to all three insecticides, especially for chlorfenapyr. Bioconcentration factors (BCFs) ranging from 0.0342 to 1.0887 were obtained, and the closer to roots, the higher BCFs. The half-life of insecticides in garlic ranged from 0.43 to 0.96 d. In the first 24 h, 55.0% - 80.3% insecticides residues in garlic were eliminated with first-order elimination kinetics. The research provides in vivo insights into the environmental fates of insecticides in complex living system with minimized organism damage.

N-doped carbon dots under Xenon lamp irradiation: Fluorescence red-shift and its potential mechanism.

Despite extensive research on carbon dots (CDs), rare studies have been performed on the photostability of CDs. Here, the photostability of CDs synthesized with 3-aminobenzoic acid were systematically investigated under different pH conditions (5.0, 7.4 and 9.0). The results showed that under Xenon lamp irradiation, the fluorescence (FL) intensity of the CDs exhibited an increase first and then a decrease, with a gradual shift of the maximum emission wavelength to longer wavelength. Further investigation indicated that the irradiation induced the change of the CD surface functional groups and gave rise to aggregation, resulting in the formation of larger particles. This study provided important reference value towards research on CDs properties.