Objective: 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. Methods: 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 rate 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. Results: 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. Conclusion: 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.
SUN Jing
,
TANG Dan-rui
,
QIANG Hui-min
,
NI Qian
,
CAO Ling
,
HANG Tai-jun
. Simultaneous determination of 43 per-and polyfluoroalkyl substances in Chinese medicinal material Pheretima by UPLC-Q Orbitrap MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2024
, 44(10)
: 1756
-1771
.
DOI: 10.16155/j.0254-1793.2024-0350
[1] 费毅琴, 肖凌, 汪波, 等. 37种植物类药材中重金属和有害元素残留分析及风险评估[J]. 药物分析杂志, 2021, 41(6):1000
FEI YQ, XIAO L, WANG B, et al. Residue analysis and risk assessment of heavy metals and harmful elements in 37 plant medicinal materials[J]. Chin J Pharm Anal, 2021, 41(6):1000
[2] SUN J, HANG T, CAO L, et al. Assessment of polybrominated diphenyl ethers and emerging brominated flame retardants in Pheretima (a traditional Chinese medicine):occurrence, residue proflles, and potential health risks[J]. Environ Pollut, 2021, 276: 116680
[3] 窦亚洁, 刘慧, 李晓萌, 等. 中药中外源性有害物的残留现状及风险评估的研究进展[J]. 中草药, 2023, 54(2):396
DOU YJ, LIU H, LI XM, et al. Research progress on residual status and risk assessment of exogenous hazardous substances in traditional Chinese medicine[J]. Chin Tradit Herb Drugs, 2023, 54(2):396
[4] 王帆, 吴婧, 庄意如, 等. 超高效液相色谱-串联质谱法测定大气中18种全氟和多氟烷基化合物[J]. 分析化学, 2023, 51(8):1371
WANG F, WU J, ZHUANG YR, et al. Determination of 18 kinds of per-and polyfluoroalkyl substances in atmosphere by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chin J Anal Chem, 2023, 51(8):1371
[5] HAMID N, JUNAID M, SULTAN M, et al. The untold story of PFAS alternatives: insights into the occurrence, ecotoxicological impacts, and removal strategies in the aquatic environment[J]. Water Res, 2024, 250: 121044
[6] XING Y, ZHOU Y, ZHANG X, et al. The sources and bioaccumulation of per-and polyfluoroalkyl substances in animal-derived foods and the potential risk of dietary intake[J]. Sci Total Environ, 2023, 905: 167313
[7] 张利娟. 中国和欧美消费品中全氟和多氟烷基物质(PFAS)合规要求分析与展望[J]. 轻工标准与质量, 2023(2):37
ZHANG LJ. Analysis and outlook on compliance requirements for perfluorinated and polyfluoroalkyl substances (PFAS) in consumer products from China and Europe and America[J]. Stand Qual Light Ind, 2023(2):37
[8] 崔建升, 杨瑞, 于玉洁, 等. 人血清中全氟和多氟烷基化合物及典型异构体的暴露特征与健康风险评估[J]. 环境科学学报, 2024, 44(2):432
CUI JS, YANG R, YU YJ, et al. Exposure characteristics and health risk assessment of per-and polyfluoroalkyl substances and their typical isomers in human serum[J]. Acta Sci Circum, 2024, 44(2):432
[9] SONG D, QIAO B, YAO Y, et al. Target and nontarget analysis of per-and polyfluoroalkyl substances in surface water, groundwater and sediments of three typical fluorochemical industrial parks in China[J]. J Hazard Mater, 2023, 460: 132411
[10] PAN YT, WANG JH, LEO W, et al. Analysis of emerging per-and polyfluoroalkyl substances: progress and current issues[J]. Trac Trend Anal Chem, 2020, 124: 115481
[11] 杨愿愿, 李偲琳, 赵建亮, 等. 超高效液相色谱-串联质谱法同时测定水、沉积物和生物样品中57种全/多氟化合物[J]. 分析化学, 2022, 50(8):1243
YANG YY, LI CL, ZHAO JL, et al. Determination of 57 kinds of per-and polyfluoroalkyl substances in waters, sediments and biological samples by ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chin J Anal Chem, 2022, 50(8):1243
[12] 齐鹏, 苏日古嘎, 杜艳青, 等. 全氟化合物的污染现状和检测技术的研究进展[J]. 化学世界, 2021, 62(3):137
QI P, SU RGG, DU YQ, et al. Progress in pollution status and determination methods of perfluorinated compounds[J]. Chem World, 2021, 62(3):137
[13] GRIFFIN EK, ARISTIZABAL-HENAO JJ, BOWDEN JA. Evaluation of different extraction methods for the analysis of per-and polyfluoroalkyl substances (PFAS) in dried blood spots from the Florida manatee (Trichechus manatus)[J]. Environ Toxicol Chem, 2021, 40(10):2726
[14] MU H, YANG Z, CHEN L, et al. Suspect and nontarget screening of per-and polyfluoroalkyl substances based on ion mobility mass spectrometry and machine learning techniques[J]. J Hazard Mater, 2024, 461: 132669
[15] OGUNBIYI OD, AJIBOYE TO, OMOTOLA EO, et al. Analytical approaches for screening of per-and poly fluoroalkyl substances in food items: a review of recent advances and improvements[J]. Environ Pollut, 2023, 329: 121705
[16] 王春兰, 张海煊, 胡望霞, 等. 气相色谱-质谱法测定纺织品中10种挥发性全氟及多氟化合物[J]. 印染, 2023, 49(4):58
WANG CL, ZHANG HX, HU WX, et al. Determination of 10 volatile per-and poly-fluorinated compounds in textiles using gas chromatography-mass spectrometry[J]. China Dye Finish, 2023, 49(4):58
[17] 孙晶, 杭太俊, 谭力, 等. GC-NCI-MS法同时测定地龙中30个溴代阻燃剂的残留量[J]. 药物分析杂志, 2020, 40(8):1425
SUN J, HANG TJ, TAN L, et al. Simultaneous determination of 30 brominated flame retardants residues in Dilong by GC-NCI-MS[J]. Chin J Pharm Anal, 2020, 40(8):1425
