UPLC-Q Orbitrap MS法同时测定中药材地龙中43个全/多氟烷基类化合物  

Simultaneous determination of 43 per-and polyfluoroalkyl substances in Chinese medicinal material Pheretima by UPLC-Q Orbitrap MS

作　　者：孙晶 唐丹瑞 强慧敏 倪倩 曹玲 杭太俊[4] SUN Jing;TANG Dan-rui;QIANG Hui-min;NI Qian;CAO Ling;HANG Tai-jun(Jiangsu Provincial Institute of Food and Drug Control,Nanjing 210019,China;School of Pharmacy,Nanjing University of Traditional Chinese Medicine,Nanjing 210023,China;Jiangsu Provincial Drug Administration Audit and Inspection Center,Nanjing 210019,China;School of Pharmacy,China Pharmaceutical University,Nanjing 211198,China)

机构地区：[1]江苏省食品药品监督检验研究院,南京210019 [2]南京中医药大学药学院,南京210023 [3]江苏省药品监督管理局审核查验中心,南京210019 [4]中国药科大学药学院,南京211198

出　　处：《药物分析杂志》2024年第10期1756-1771,共16页Chinese Journal of Pharmaceutical Analysis

基　　金：江苏省药品监督管理局科研计划项目(编号202205)。

摘　　要：目的:建立地龙药材中43个痕量多残留全/多氟烷基类化合物(PFAS)的UPLC-Q Orbitrap MS同时测定方法。方法:地龙药材,加氯化钠和多种同位素内标,经含0.2%甲酸乙腈超声20 min结合高速振荡10 min提取;冷冻离心,分取上清液,浓缩至约0.5 mL,加含0.05%甲酸的40%甲醇水溶液5 mL,混合均匀;经混合型弱阴离子交换固相萃取柱(6 mL,150 mg)净化;以甲醇和0.5%氨水甲醇各3 mL依次洗脱,收集洗脱液,氮气吹至近干,分别以0.5 mL甲醇复溶,冷冻离心后取上清液,采用超高效液相色谱-四极杆/静电场轨道阱质谱(UPLC-Q Orbitrap MS)法对地龙药材中43个PFAS进行同时测定。色谱-质谱条件:采用ACE EXCEL 2 C_(18)(150 mm×2.1 mm,2μm)色谱柱分离,以5 mmol·L^(-1)甲酸铵溶液-乙睛为流动相,梯度洗脱,流速0.3 mL·min^(-1),柱温35℃,进样体积2μL;电喷雾负离子化四极杆/静电场轨道阱质谱法m/z 100~1000全扫描检测,提取目标离子内标法定量。结果:43个PFAS同时测定,专属性强,线性关系良好(r>0.995),加样回收率在68.3%~121.4%,重复性RSD为3.5%~15.0%,检测限和定量限分别为0.01~0.15μg·kg^(-1)和0.02~0.5μg·kg^(-1)。20批地龙样品中,共检出22个PFAS痕量残留。结论:建立的地龙药材中43个PFAS痕量残留的UPLC-Q Orbitrap MS同时测定法灵敏准确,适用于地龙和基质相似中药材中PFAS的日常监测,及其质量风险的评估与控制。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 C_(18)chromatography column(150 mm×2.1 mm,2μm),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 2μL.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 100-1000.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 0.01-0.15μg·kg^(-1)and 0.02-0.5μg·kg^(-1).respectively.A total of 22 kinds of PFAS were de

关 键 词：地龙 全/多氟烷基类化合物 新污染物 中药 超高效液相色谱-四极杆/静电场轨道阱质谱 固相萃取 6∶2氟调磺酸 F-53铬雾抑制剂 

分 类 号：R917[医药卫生—药物分析学]