Determination Of Plant Growth Regulators And Granisetron Hydrochloride By Tandem Mass Spectrometry

Now people pay more attention to the safety of drugs and food.Therefore,developing an efficient quantitative detection method with high sensitivity and high selectivity is extremely urgent.Due to its high sensitivity and selectivity,the HPLC-MS/MS technique has become a research focus,which has a wide range of application in the quantitative study of determination of chemicals in drugs,food and environment.This paper adopted triple quadrupole mass spectrometer and developed a method of the detection of plant growth regulators in the batatas and a method of the detection of granisetron hydrochloride in beagle dog's plasma.For the analysis of plant growth regulators,the pretreatment method based matrix solid-phase dispersive(MSPD)could shorten the extraction time.However,there is a lack of testing in tubers and a lack of optimization studies on pretreatment.For the analysis of granisetron hydrochloride,the traditional reversed-phase liquid chromatography has a weak retention problem,which is not conducive to the accuracy of the integration.To solve these problems,the following research has been carried out in this thesis.A sample pretreatment method based on the matrix solid-phase dispersive(MSPD)extraction was developed for the determination of forchlorfenuron?6-BA?MGK-264 and paclobutrazol in batatas.Samples were ground with silica,extracted with methanol..The batatas samples were ground with dispersant materials,and then extracted with methanol.Coupled with the optimized MSPD pretreatment,a liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)analysis method was established to detect the plant growth regulators,using selecting reaction monitoring(SRM)detection mode,and the quantification was performed using external standard.This method was evaluated by matrix effect and recovery.The linear correlation coefficient of forchlorfenuron,paclobutrazol,MGK-264 and 6-BA were more than 0.9,and the limits of quantitation(LOQs)were around 0.1 ng/g ~ 0.5 ng/g.The spiked recoveries of four plant growth regulators at levels of 50 ng/g,100 ng/g and 200 ng/g of plant growth regulators were in the range of 70% ~ 135%.A sample pretreatment method based on the matrix solid-phase dispersive(MSPD)extraction was developed for the determination of forchlorfenuron in batatas.Based on dispersant materials of hydrophobic showed good retention for forchlorfenuron,batatas samples were ground with C18 HC,and then extracted with methanol.Coupled with the optimized pretreatment,selecting reaction monitoring(SRM)was used to detect samples.The quantification was performed using external standard.This method was evaluated by matrix effect and recovery.The linear correlation coefficient of forchlorfenuron was more than 0.9.The spiked recoveries of forchlorfenuron at levels of 10 ng/g,25 ng/g and 50 ng/g of forchlorfenuron were in the range of 70% ~ 130%.A sample pretreatment method based on liquid-liquid extraction extraction was explored for the determination of granisetron hydrochloride in beagle dogs' plasma.A liquid-liquid extraction coupled with hydrophilic interaction liquid chromatography–tandem mass spectrometry was developed,and the quantification was performed using internal standard.The chromatography separation mode and conditions were investigated and optimized.This method was systematically evaluated,and the linear ranges of granisetron hydrochloride were between 0.11 ng/m L and 11.00 ng/m L with the linear correlation coefficient more than 0.9.The limit of quantitation(LOQ)of the granisetron hydrochloride was 0.06 ng/m L.The spiked recoveries at levels of 0.11 ng/mL,1.10 ng/m L and 6.60 ng/mL of granisetron hydrochloride were in the range of 56% ~ 70%.