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To establish an UPLC-Q Orbitrap MS determination method for multiple residues of exogenous new pollutants，per-and polyfluoroalkyl substances (PFAS)，in Pheretima medicinal materials.
The samples were extracted with acetonitrile (containing 0.2% formic acid) after adding sodium chloride and 27 isotopes labeled internal standard solutions. Ultrasound treatment was performed for 20 min，followed by high-speed oscillation for 10 min. The extraction solution was subjected to freeze centrifugation，and the supernatant was concentrated to about 0.5 mL. Then，5 mL of 40% methanol (containing 0.05% formic acid) was added and mixed well. Further purified by mixed weak anion exchange solid-phase extraction (6 mL，150 mg)， eluted sequentially with 3 mL of methanol and 3 mL of 0.5% ammonia water methanol，and the eluents were collected，respectively. After blowing the eluent nitrogen to near dryness，the residue was redissolved in methanol，and the supernatant was taken for instrumental analysis after freezing and centrifugation. The target and internal PFAS were separated on an ACE EXCEL 2 C18 chromatography column (150 mm×2.1 mm，2 μm)，using 5 mmol·L-1 ammonium formate solution and acetonitrile were used as the mobile phase for gradient elution. The flow rat e was set to 0.3 mL·min-1，the column temperature was 35 ℃，and the injection volume was 2 μL. The PFAS were detected by UPLC-Q Orbitrap MS in negative electrospray ionization mode with full scanning monitoring with the scanning range of m/z 100-1 000. Quantification of 43 PFAS using internal standards was performed based on their peak areas in extract ion chromatogram.
The method had good specificity，with a good linear relationship between the 43 tested indicator components and correlation coefficients greater than 0.995. The recovery rate of all indicators for sample addition was 68.3%-121.4%，the repeatability was 3.5%-15.0%. The detection limits and quantification limits were 0.01-0.15 μg·kg-1 and 0.02-0.5 μg·kg-1. respectively. A total of 22 kinds of PFAS were detected in 20 batches of Pheretima samples.
The UPLC-Q Orbitrap MS method is sensitive and accurate for simultaneous determination of 43 trace and multiple residual PFAS in Pheretima medicinal materials. It is suitable for daily monitoring of PFAS in Chinese medicinal materials with similar matrices，as well as assessment and control of quality risks.
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| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |
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