Field investigations on perfluoroalkyl acid (PFAA) levels in various environmental matrixes were reported, but there is still a lack of PFAA level data for agricultural environments, especially agricultural producing areas, so we collected soil, irrigation water and agricultural product samples from agricultural producing areas in the provinces of Liaoning, Shandong and Sichuan in China. The background pollution from instruments was removed and C4–C18 PFAAs were detected by LC-MS/MS. The concentrations of PFAAs in the top and deep layers of soil were compared, and the levels of PFAAs in different agricultural environments (greenhouses and open agriculture) were analyzed. We found the order of PFAA levels by province was Shandong > Liaoning > Sichuan. A descending trend of PFAA levels from top to deep soil and open to greenhouse agriculture was shown and perfluorobutanoic acid (PFBA) was considered as a marker for source analysis. Bean vegetables contribute highly to the overall PFAA load in vegetables. A significant correlation was shown between irrigation water and agricultural products. The EDI (estimated daily intake) from vegetables should be of concern in China.
This study established an effective analytical method for the direct simultaneous determination of GLY, N -acetyl-GLY, AMPA, N -acetyl-AMPA, GLU, NAG, and 3-MPPA in soybean and maize, which will contribute to the scientific regulation of GLY and GLU.
In this study, a simple, rapid and sensitive method was developed for the simultaneous determination of chlormequat, fosetyl-aluminium and phosphonic acid residues in maize and soybean using liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS). Analytes were extracted with acetic acid solution, purified on an HLB column, and then filtered through a 0.2 μm hydrophilic microporous filter membrane. They were then separated on an IC column using a separation phase consisting of polyvinyl alcohol particles with quaternary ammonium groups. The mobile phase optimised with water was denoted as mobile phase A and that optimised with 200 mmol L−1 ammonium bicarbonate solution containing 0.05% ammonium hydroxide was denoted as mobile phase B. The residues were detected by tandem mass spectrometry with negative electrospray ionization in a multi-reaction monitoring mode. The correlation coefficient (R ≥ 0.997) showed good linear regressions for all analytes in water as well as in maize and soybean matrices with a wide dynamic range of 0.001 to 0.5 mg L−1 for calibration. The mean recoveries (RSDs) of the analytes were in the range 85.0–106.4% (5.5–14.9%), 81.7–109.5% (2.7–11.0%) and 74.7–104.4% (2.9–6.1%) at three concentration levels (0.05, 0.1 and 1 mg kg−1) for the interday test (n = 15). The limit of quantification (LOQ) and detection (LOD) of the method for different matrices were 0.01 and 0.003 mg kg−1, respectively. In conclusion, the established analytical approach has high sensitivity and good accuracy and precision and is suitable for monitoring chlormequat, fosetyl-aluminium and phosphonic acid residues in maize and soybean.