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

Determination of Dithiocarbamates in Foodstuffs by LC-MS/MS

通过优化质谱、液相色谱和萃取缓冲液等条件,建立了一种简单、快速、灵敏测定食品中二硫代氨基甲酸酯的方法。在优化条件下,代森锌(EbdC)、丙森锌(PbdC)的线性范围为2~100μg/l,相关系数均不小于0.997。在花椰菜、萝卜和豌豆中EbdC和PbdC的检出限(S/n>3)为2μg/kg;萝卜和豌豆中Eb-dC和PbdC的定量下限(S/n>10)为10μg/kg,而花椰菜中EbdC和PbdC的定量下限(S/n>10)为15μg/kg。在花椰菜、萝卜和豌豆基质中加标5~100μg/kg的EbdC和PbdC时,测定加标回收率为83%~96%,相对标准偏差为4.4%~10.5%,方法可满足定量分析的要求。A simple,fast and sensitive method was developed for the determination of dithiocarbamates,including tiezene(EBDC) and pestanal(PBDC),by optimizing the parameters of LC-MS/MS and extraction buffer.Under the optimized conditions,the calibration curves of EBDC and PBDC were linear in the range of 2-100 μg/L with correlation coefficients not less than 0.997.The limits of detection(LODs,S/N>3) of EBDC and PBDC were 2 μg/kg for cauliflower,turnip and pea,and the limits of quantitation(LOQs,S/N>10) of EBDC and PBDC were 10 μg/kg for turnip and pea,and 15 μg/kg for cauliflower.The recoveries in cauliflower,turnip and pea samples at spiked concentration levels of 5-100 μg/kg ranged from 83% to 96% with relative standard deviations(RSDs) of 4.4%-10.5%.The method could meet the requirement for the analysis of dithiocarbamates in foodstuffs.厦门市科技计划项目(3502Z20092009;3502Z20102013); 国家质检总局科技计划项目(2010IK162;2010IK192

连续含铝SiC自由膜的制备与发光特性研究

通过自制喷膜装置对聚铝碳硅烷(PACS)进行脱泡处理、熔融纺膜,并对其进行氧化交联、高温预烧及高温裂解终烧可制得连续含铝SiC自由薄膜。用扫描电镜(SEM)分析薄膜的形貌,通过红外光谱(FT-IR)分析氧化交联后薄膜的结构变化,通过电子探针(EPMA)、拉曼光谱(Raman)、X射线衍射(XRD)与场发射高分辨透射电子显微镜(HRTEM)对薄膜进行成分及微观结构分析,采用光致发光谱(PL)对薄膜的光学带隙和发光特性进行了研究。结果表明,熔融纺膜法与PACS先驱体法相结合可制得均匀、致密的耐高温连续含铝SiC自由薄膜,室温下表现出了320~440nm宽谱带发光,其发光峰可分别归因于-αSiC和C簇,且随着烧结温度的提高,发光强度增大

トマト栄養診断技術のための葉柄汁液試料の調整法の検討(農学)

わが国の養液栽培における栄養診断技術の確立と普及を目的に, 簡易で迅速な無機養分の汁液分析法の試料の抽出, 調整法について検討した。葉柄組織の磨砕による汁液の抽出方法として, 作業が楽で, 迅速でしかも磨砕程度の再現性が高いホモジナイザーが優れていると判断した。葉1枚から採取する葉柄重量が3g程度のわずかな量で測定できることがわかった。汁液の脱色のために使用する活性炭については, 種類も添加時期も汁液中の無機養分濃度の測定値に及ぼす影響が認められなかった。原子吸光法による汁液中のCa濃度の測定では, 塩化ストロンチウム無添加では栄養診断上, 支障となる程度の濃度低下がおこることがわかった。The quick and easy technique of petiole sap analysis of tomato grown in hydroponics was discussed. Extraction by homoginizer was better than by mortar in that homoginizer method was less laborious and constant results were obtained. Three grams tissue of main petiole of tomato leaf was enough for nutrient analysis. Addtion of activated carbon powder for the purpose of discoloration was not necessary for phosphate measurement by photometer. The value of Ca concentration measured by atomic absorption spectrometer without SrCl_2 was aparrently lower than that with addition of SrCl_2

THE DISCUSSION AND PRACTICE OF A TEACHING MODEL OF ADOPTING THE SMALLSCALE TO SEMIMICRO SCALE TO MICROSCALE REACTION IN ORGANIC CHEMISTRY LAB.

本文介绍了小量—半微量—微量有机化学实验的教学内容和特点 ,及在教学中初步试用的效果Smallscale semimicro microscale organic experiments have been practised step by step.It benefits the reform of teaching model of experiment course and enhances the quality of chemistry teaching

老年人脑腔隙梗死与胰岛素抵抗关系的临床研究

目的探讨老年人脑腔隙梗死(腔梗)与胰岛素抵抗(IR)的关系。方法对354例受试者行空腹血糖(FPG)、甘油三脂(TG)、总胆固醇(TC)、高密度脂蛋白胆固醇(HDL-C)、低密度脂蛋白胆固醇(LDL-C)检测。采用放免法测定空腹胰岛素(FIN)。评估机体胰岛素抵抗(HOMA-IR),并计算其体重指数(BMI)。将腔梗组按无、有高血压及高 TG/低 HDL 分为Ⅰ、Ⅱ两组。结果腔梗组与健康对照组比较 TG,TC、LDL、FIG、FIN、HOMA-IR 有非常显著差异(P<0.01)。在校正年龄、性别、BMI 后老年人腔梗仍有显著的 IR,且不受高血压和高 TG 的影响。结论老年人腔梗较健康老人有明显的 IR。高 TG、高 LDL、IR 是影响老年人腔梗的可能是独立的危险因素,老年人腔梗与 IR 关系密切,呈正相关