Fast Screening of 5 Polar Poisons in Blood Sample by Paper Capillary Spray Tandem Mass Spectrometry
  
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KeyWord:paper capillary spray  ?ambient ionization  ?polar compounds  ?blood sample
  
AuthorInstitution
ZHANG Yun-feng,DONG Lin-pei,ZHAO Sen,SUN Long,CHANG Jing,REN Xin-xin,WANG Ai-hua 1. Institute of Forensic Science,Ministry of Public Security,Beijing ,China;2. Zhejiang Police College,Hangzhou ,China;3. PURSPEC Technologies,Beijing ,China
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Abstract:
      A fast screening method was developed for the analysis of five extremely polar poisons in whole blood sample using paper capillary spray(PCS) tandem mass spectrometry.The five extremely polar poisons are diquat,paraquat,glyphosate,glufosinate-ammonium and succinylcholine chloride.The whole blood sample was extracted with methanol,at a ratio of 1 to 9(by volume) for sample and methanol.After mixing the sample and keeping it static,100 μL supernatant was loaded onto the paper capillary spray cartridge.The cartridge was then inserted into the inlet of PURSPEC MS Mate interface,which was coupled to a Shimadzu 8040 tandem mass spectrometry system.Afterwards,the analytes were directly analyzed qualitatively and quantitatively using the two precursor ion-product ion pairs with multiple reaction monitoring(MRM) mode.With the help of no complicated sample preparation provided by PCS cartridge as an ambient ionization technique,together with the direct coupling of PCS to commercial instrument by MS Mate,the five polar targets could be detected within 1 minute,which is much faster than current methods.During the research process,the mass spectrometry parameters were optimized first,and the ion pairs for each analyte were found with their corresponding standard solutions.The qualitative and quantitative ion pairs are listed as follows:diquat(positive mode,183.1?> 157.0*,183.1 > 130.0),paraquat (positive mode,185.1 > 170.1,186.1 > 171.1*),glyphosate(negative mode,168.0 > 63.0,168.0 > 150.0*),glufosinate-ammonium(negative mode,180.1 > 85.0*,180.1 > 136.0),and succinylcholine chloride (positive mode,145.1 > 93.6,145.1 > 115.5*),where the ion pairs with the asterisk refer to quantitative ion pairs. The limits of detection(LODs) for the five polar compounds in blood sample were 0.05 mg/L for diquat,0.5 mg/L for paraquat,25 mg/L for glyphosate,25 mg/L for glufosinate-ammonium,and 0.05 mg/L for succinylcholine chloride.Here the definition of signal-to-noise(S/N) ratio no less than 3 was used for LOD measurement.Linearity was measured by spiking analyte standards to the methanol extracted supernatant from blank blood sample.Good linearity was achieved in the range of 0.005-0.5 mg/L for diquat and succinylcholine chloride,in the range of 0.05-5 mg/L for paraguat,and in the range of 2.5-100 mg/L for glyphosate and glufosinate-ammonium.The spiked recovery ranged from 62% to 117% with relative standard deviation less than 40% under 1,2,10 times detection limit.Using the method developed in this article,whole blood samples from poisoned patients were analyzed and the corresponding poisons were correctly identified and quantified,which shows that the performance of the PCS-MS Mate-MS/MS method meets the need in real life for fast screening analysis.The method is convenient and suitable for the fast screening of polar poisons in blood samples.
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