Determination of Chlorpromazine and Promethazine and Their Metabolites in Animal Food Using Ultra Performance Liquid Chromatography with Tandem Mass Spectrometry

建立了动物源食品中吩噻嗪类药物氯丙嗪、异丙嗪及其代谢物氯丙嗪亚砜和异丙嗪亚砜同时测定的固相萃取超高效液相色谱-电喷雾电离串联四极杆质谱(uPlC-ESIMS/MS)方法。样品用乙酸乙酯和氢氧化钠溶液提取,OASIS Hlb柱富集净化,超高效液相色谱-电喷雾串联四极杆质谱仪检测,采用多反应监测正离子模式,可以一次性对动物源性食品中的吩噻嗪类药物氯丙嗪、异丙嗪及其代谢物氯丙嗪亚砜和异丙嗪亚砜进行定性和定量测定。方法在1--100μg/l范围具有良好的线性,回收率为76%--96%,定量下限(S/n>10)为异丙嗪5μg/kg,氯丙嗪、氯丙嗪亚砜、异丙嗪亚砜1μg/kg。检出限(S/n=3)为异丙嗪1.5μg/kg,氯丙嗪、氯丙嗪亚砜、异丙嗪亚砜0.3μg/kg。A method for the simultaneous detection residues of chlorpromazine and promethazine and their metabolites chlorpromazine sulphoxide and promethazine sulphoxide in animal foods was developed by using solid phase extraction(SPE) combination with ultra performance liquid chromatography-electrospray ionization triple-quadruple tandem mass spectrometry(UPLC-ESI MS/MS).The chlorpromazine and promethazine and their metabolites in the test sample was extracted with ethyl acetate and sodium hydroxide solution.The homogenate was centrifuged and the supernatant was collected.The extract was cleaned up and concentrated on an Oasis HLB cartridge,and then analyzed by UPLC-ESI MS/MS under the positive ion mode using multiple reaction monitoring(MRM) mode.Extraction and chromatographic conditions were optimized and the best separation was obtained.The cabalibration curves were linear in the range of 1-100 μg/L.The average recoveries were between 76% and 96%(n=6) in the spiked range of 5-100 μg/kg in pork,fish,dullfrog and milk.The limits of quantification(S/N>10) were in the range of 1-5 μg/kg and the limits of detection(S/N=3) were 0.3-1.5 μg/kg.国家质量监督检验检疫总局科研计划资助项目(2007IK137

基于UPLC-oaTOF-MS的糖尿病及糖尿病肾病的代谢组学研究

Ultra performance liquid chromatography(UPLC) coupled with orthogonal acceleration time-of-flight(oaTOF) mass spectrometry is becoming an effective and high-throughput analytical technique in metabonomics research.In this paper,an UPLC-oaTOF-MS system was employed to investigate the serum profiles of 40 diabete mellitus(DM)/diabetic nephropathy(DN) patients and 25 healthy volunteers in an effort to find potential biomarkers.The UPLC system produced information-rich chromatograms with typical measured peak widths of 4 s,and generated peak capacities of 225 in 15 min.After the UPLC-oaTOF-MS analysis,principal component analysis(PCA) was used for group differentiation and marker selection.In the projection of positive mode,DM/DN patients and the controls were obviously divided into three groups.Furthermore,two potential markers were identified as phytosphingosine and sphinganine,respectively.Phytosphingosine and sphinganine with decreased concentrations in the patients,were closely related to the sphingolipid me..

Metabonomics Research of Diabetes Mellitus and Diabetic Nephropathy Based on UPLC-oaTOF-MS System

Ultra performance liquid chromatography (UPLC) Coupled with orthogonal acceleration time-of-flight( (oaTOF) mass spectrometry is becoming an effective and high-throughput analytical technique in metabonomics research. In this paper, an UPLC-oaTOF-Ms system was employed to investigate the serum profiles of 40 diabete mellitus(DM)/diabetic nephropathy(DN) patients and 25 healthy volunteers in an effort to find potential biomarkers. The UPLC system produced information-rich chromatograms with typical measured peak widths of 4 s, and generated peak capacities of 225 in 15 min. After the UPLC-oaTOF-MS analysis, principal component analysis (PCA) was used for group differentiation and marker selection. In the projection of positive mode, DM/DN patients and the controls were obviously divided into three groups. Furthermore, two potential markers were identified as phytosphingosine and sphinganine, respectively. Phytosphingosine and sphinganine with decreased concentrations in the patients, were closely related to the sphingolipid metabolism

JUNO Sensitivity on Proton Decay p→νˉK+p\to \bar\nu K^+ Searches

The Jiangmen Underground Neutrino Observatory (JUNO) is a large liquid scintillator detector designed to explore many topics in fundamental physics. In this paper, the potential on searching for proton decay in $p\to \bar\nu K^+$ mode with JUNO is investigated.The kaon and its decay particles feature a clear three-fold coincidence signature that results in a high efficiency for identification. Moreover, the excellent energy resolution of JUNO permits to suppress the sizable background caused by other delayed signals. Based on these advantages, the detection efficiency for the proton decay via $p\to \bar\nu K^+$ is 36.9% with a background level of 0.2 events after 10 years of data taking. The estimated sensitivity based on 200 kton-years exposure is $9.6 \times 10^{33}$ years, competitive with the current best limits on the proton lifetime in this channel