The Applications Of Liquid Chromatography-Triple Quadrupole Mass Spectrometry With On-line Solid Phase Extraction In Analysis Of Three Types Of Medicines

In recent years,drug abused and illegal drug used have emerged.Due to the development of synthetic drug industry,the development of all kinds of new drugs are altering from day to day,which brings great difficulties to clinical treatment and forensic toxicology analysis.Forensic toxicology analysis is a qualitative and quantitative applied discipline based on modern instrument analysis.It provides reasonable clues and powerful evidence for cases related to toxicants.It's a great challenges for the detection,because the subjects of forensic toxicology analysis are mainly biological materials,such as blood,urine,saliva,body tissues,etc.The matrix composition is complex,and the content of analyte in the samples is very low.A liquid chromatography-triple quadrupole mass spectrometry(LC-MS/MS)with on-line solid phase extraction(on-line SPE)method was developed and validated for the simultaneous determination of three types forensic toxicants in biological samples.The pretreatment of samples is highly automated and easy to operate.On-line SPE greatly reduces the pretreatment time.The method is was simple,reliable and high sensitive.It provides an effective technical support for clinical treatment and forensic toxicology analysis,which has important guiding significance.(1)A method of liquid chromatography-triple quadrupole mass spectrometry(LC-MS/MS)with On-line SPE for the simultaneous determination of 10 barbiturates in blood and urine was developed and validated.The samples were treated with acetonitrile,and then purified by a column with polymer of hydrophilic-lipophilic balance(HLB),then directly detected by MS/MS.The analytes were detected in multiple reaction monitoring(MRM)mode under negative electrospray ionization mode(ESi-)and quantified by external standard method.The results showed that the correlation coefficients were>0.9988 within the investigated mass concentration ranges of the 10 barbiturates.The LODs varied from 10.0 ng·mL-1(ng·g-1)to 20.0 ng·mL-1(ng·g-1),and the LOQs varied from 20.0 ng·mL-1(ng·g-1)to 50.0 ng·mL-1/(ng·g-1).(2)A liquid chromatography-triple quadrupole mass spectrometry(LC-MS/MS)with on-line SPE method was developed and validated for the simultaneous determination of benzodiazepines and metabolites in whole blood,urine and liver tissue samples.The samples were protein precipitated with acetonitrile,and purified by a column with HLB,then directly detected by MS/MS.The analytes were detected in DMRM mode under ESI+ and quantified by external standard method.The results showed that the correlation coefficients were not less than 0.9984 within the investigated mass concentration ranges of the forty drugs by quadratic equation fitting.The LODs varied from 0.01 ng·mL-1(ng·g-1)to 1.00 ng m·L-1(ng·g-1),and the LOQs varied from 0.10 ng·mL-1(ng·g-1)to 10.0 ng·mL-1(ng·g-1).This method was simple,reliable and high sensitive.The application of the proposed method using on-line solid phase extraction in a forensic toxicological analyses was successful.(3)A liquid chromatography-triple quadrupole mass spectrometry(LC-MS/MS)with on-line SPE method was developed and validated for the simultaneous determination of ninety organophosphorus pesticides in whole blood and liver tissue samples.The samples were protein precipitated with acetonitrile,and purified by a column with HLB,then directly detected by MS/MS.The analytes were detected in DMRM mode under ESI+ and quantified by external standard method.The results showed that the correlation coefficientswere not less than 0.9990 within the investigated mass concentration ranges of the ninety drugs by quadratic equation fitting.The LODs varied from 0.01 ng·mL-1(ng·g-1)to 5.00 ng·mL-1(ng·g-1),and the LOQs varied from 0.02 ng·mL-1(ng·g-1)to 10.0 ng·mL-1(ng·g-1).