A method for determination of fatty acids(FA) compositions in human serum by gas chromatography time-of flight mass spectrometry(GC-TOF MS) method was established.The FA in serum were directly transformed into the fatty acid methyl esters by 2.5% H2SO4-methanol.Heptadecanoic acid methyl esters were used as internal standard.The detection and separation of all the FA were performed within 33 min.The established method has the characteristic of simple operation,rapid analysis,high accuracy,large amount of information and safety.So it is suitable for the scientific research to the disease correlating FA.
目的:采用高效液相色谱法(HPLC)建立雪莲培养物指纹图谱。方法:以紫丁香苷为参照物,采用梯度洗脱HPLC法建立雪莲培养物指纹图谱,并进行相似度评价和聚类分析。色谱柱为CAPCELL PAK C18(4.6 mm×250mm,5μm),流动相A为0.1%TFA/水,流动相B为0.1%TFA/乙腈,梯度洗脱,检测波长260 nm。结果:建立了雪莲培养物指纹图谱,方法的精密度、稳定性、重现性较好,共标示出9个共有峰。结论:该法为雪莲培养物的鉴定提供了依据,其指纹图谱可用于雪莲培养物的质量控制。
To establish HPLC electrospray ionization mass spectrometry (HPLC-ESI MS) method for determination of osthole in food additive.The samples were dipped in methanol overnight and extracted with it by ultrasonic instrument,then the supernatant was send to sampler for detection.Sample was chromatographed using 0.4%HAc solution-MeOH (35:65,by volume) mobile phase on an Xterra MS C18 column.Analyte determination was performed by ESI MS/MS in the multiple reaction monitoring(MRM)mode.The established method of LC-MS/MS determining the concentration of osthole in food additive has the characteristic of strong specificity,high sensitivity and good reproducibility.The linear range of papaverine was 0.001-10 μg/mL,method recovery was 97.42%,RSD was 8.37%,the limit of detection was 1 ng/mL and the limit of quantitation was 0.001 μg/mL.
Liquid chromatography-mass spectrometry(LC-MS) was combined by high resolution of high-liquid chromatography and high sensitivity,high specificity of mass spectrometry,which not only can separate the complicated mixtures,but also doesn’t need more complicated pre-treatment for samples.The qualitative and quantitative analysis of quercetin was implemented by the information of the molecular structure and fragment.In this paper,the LC-MS/MS method was established for determination of quercetin in plasma.
