Pesticide residues in aquatic products are of great concern due to the risk of environmental transmission and their extensive use in aquaculture. In our work, a quick screening approach was developed for the qualitative and semi-quantitative screening of 87 pesticide residues in aquatic products. The sample preparation was investigated, including extract solvent, extract methods, buffer salts, lipid removal, cleanup materials and filter membranes for aquatic products. Samples were extracted using a modified QuEChERS procedure, and two clean-up procedures were developed for UHPLC-Q/Orbitrap MS analysis based on the fat content of the aquatic products. The screening detection limits for all studied pesticides were distributed between 1 and 500 μg/kg in the three representative matrices. Seventy-one pesticides could be analyzed with a screening limit between 1 and 25 μg/kg in grass carp and crayfish, sixty-one pesticides could be screened for limits between 1 and 50 μg/kg in crab. The accuracy results showed that recoveries ranged from 50 to 120% for 60, 56 and 52 pesticides at medium-level for grass carp, crayfish and crab, respectively. At high spiking levels, 74, 65 and 59 pesticides were recovered within the range of 50–120% for the three matrices, respectively. The relative standard deviations of most compounds in different matrices were less than 20%. With this method, the local farmed aquatic products were tested for pesticide residues. In these samples, ethoxyquinoline, prometryn and phoxim were frequently detected. The majority of these confirmed compounds did not exceed 2.00 μg/kg. A grass carp with trichlorfon at 4.87 μg/kg and two carps with ethoxyquinoline at 200 µg/kg were detected, indicating the potential dietary risk.

Multiclass screening of drugs with high resolution mass spectrometry is of great interest due to its high time-efficiency and excellent accuracy. A high-scale, fast screening method for pesticides in fishery drugs was established based on ultrahigh performance liquid chromatography tandem quadrupole-Orbitrap high-resolution mass spectrometer. The target compounds - were diluted in methanol and extracted by ultrasonic treatment, and the extracts were diluted with MeOH-water (1:1, v/v) and centrifuged to remove impurities. The chromatographic separation was performed on an Accucore aQ-MS column (100 mm × 2.1 mm, 2.6 μm) with gradient elution using 0.1% formic acid in water (containing 5 mmol/L ammonium formate) and 0.1% formic acid in methanol (containing 5 mmol/L ammonium formate) in Full Scan/dd-MS2 (TopN) scan mode. A screening database, including mass spectrometric and chromatographic information, was established for identification of compounds. The screening detection limits of methods ranged between 1–500 mg/kg, the recoveries of real samples spiked with the concentration of 10 mg/kg and 100 mg/kg standard mixture ranged from 70% to 110% for more than sixty compounds, and the relative standard deviations (RSDs) were less than 20%. The application of this method showed that target pesticides were screened out in 10 samples out of 21 practical samples, in which the banned pesticide chlorpyrifos were detected in 3 out of the 10 samples.

This study described the development of a multiresidue method based on gas chromatography (GC) for the detection of 7 indictor polychlorinated biphenyls (PCBs) and 13 organochlorine pesticide (OCPs) residues in sediment with electron capture detector (ECD). The samples were extracted by n-hexane/dichloromethane (1/1, v/v) by ultrasonic extraction. The extracts were desulfurization with copper powder and purification with concentrated sulfuric acid. The method was validated by the analysis of spiked Tai lake sediment. Analytical performances were evaluated in terms of linearity, quantification limits, accuracy, and precision. Good linearity responses with coefficients of determination higher than 0.9945 were obtained. Methodological limit of quantitation (LOQ) was 0.5-5.0μg/kg for OCPs and PCBs. The recovery and RSDs of three-level spiked samples were in the ranges of 71.6%-105% and 3.2-11.2%. This method is highly effective to reduce the cost and time for the pretreatment of sample, and offers the ability to detect and quantify the PCBs and OCPs in sediments.