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Study And Application Of Qualitative And Quantitative GC-MS Detection Of Amphetamine And Diazepam Psychotropic Drugs In Hair

Posted on:2020-07-28Degree:MasterType:Thesis
Country:ChinaCandidate:Y L M M T MaFull Text:PDF
GTID:2404330572481733Subject:Public health
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Objective:to establish a method for the detection of phenylalanine and valium in human hair by GC-MS.A qualitative and quantitative detection method with simple pretreatment,high extraction rate,high sensitivity and fast analysis speed was established.Methods:benzedrine in hair and antipsychotic drugs,under the condition of PH10?11to5ml Extrelut3 miniature solid phase extraction column solid-phase extraction,SKF525a as internal standard,respectively by formic acid chloride 2,2,2-cross-linked ethyl ester(3clec)and double methyl silane three fluoroacetamide(BSTFA)as the derivatization reagent,using HP-5 MS polarity of chromatographic column GC-MS method Full Scan and SIM for quantitative analysis.Results:Results(1)the minimum detection limit of 8amphetamines in hair was 3ng/mg,and the minimum quantitative limit was 30ng/mg.R~2>0.9902,average recovery 99.11?103.54,accuracy(SD)0.21?13.37,precision(RSD)0.24?7.28.(2)The derivative effects of 3Clec,BSTFA and HFBA were compared,and the results showed that the use of 3Clec derivative reagents had the highest recovery rate and the best derivative effect for amphetamines in hair.(3)Univariate analysis showed that the recovery rate of 8 amphetamines in hair treated with 3Clec derivative reagent was higher than that without derivative reagent(P<0.05).The recovery of SPE was higher than that of LLE,and the difference was statistically significant(P<0.05).(4)The minimum detection limit of 14 antipsychotic drugs in hair was 3ng/mg,and the minimum quantitative limit was 30ng/mg.The standard curve was made within the linear range,and the standard curve presented a good linear relationship.R~2>0.9901,average recovery was82.05?100.74%,accuracy(SD)was 0.03?6.19,precision(RSD)was 0.05?9.19.(5),according to the results of single factor analysis of 14 kinds of antipsychotic drugs in hair clonazepam,lorazepam,diazepam,nitrate,the sand to point a diazepam diazepam,temazepam 6 kinds of antipsychotic drugs by BSTFA derived after the recovery rate is higher than the recovery,the derivative of the and statistically significant difference(P<0.05),and other eight kinds of antipsychotic drugs there was no statistically significant difference before and after derivatization recovery;The recovery of 14 kinds of antipsychotic drugs in hair pretreatment by solid phase extraction was higher than that by liquid-liquid extraction,and the difference in recovery was statistically significant(P<0.05).(6)Hair samples of the case were tested by the established method.In the first case,methamphetamine was detected at 26.36ug/mL.In the second case,temazepam with a content of 14.54ug/mL and prazepam with a content of 25.36ug/mL were detected.Conclusion:The precision,accuracy and detection sensitivity of this method are high,quasi-deterministic and quantitative,suitable for qualitative and quantitative detection of amphetamine and diazepam in hair.
Keywords/Search Tags:Amphetamines, Diazepam, Hair, Solid phase extraction, Derivatization, GC-MS
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