超高效液相色谱-串联质谱法同时快速测定食用油中9种外源性杂质成分

建立了超高效液相色谱-串联质谱同时快速测定食用油中9种外源性杂质成分的分析方法。样品经乙腈涡旋提取后,采用XSelect~?HSS PFP(100 mm×2.1 mm,3.5μm)色谱柱,以5 mmol/L甲酸铵-乙腈为流动相进行梯度洗脱,在10 min内实现9种待测物的良好分离。在电喷雾正离子模式下,以多反应监测(MRM)模式采集数据并作定性鉴别和定量分析。结果表明,9种待测物在相应的质量浓度范围内线性关系良好,相关系数(r~2)均大于0.996;在3个不同浓度加标水平下,平均回收率为68.2%～104%,相对标准偏差(RSD)为2.2%～12%,检出限(LOD,S/N≥3)和定量下限(LOQ,S/N≥10)分别为0.02～0.10μg/kg及0.05～0.25μg/kg。结果表明,该法简单、快速、灵敏、准确、可靠,适用于食用油中9种难挥发外源性特征杂质的同时快速定性和定量分析。     

紫穗槐叶中杀虫化学成分的分离和结构鉴定

紫穗槐[Amorphafruticosa(L)]是豆科紫穗槐属植物中的一种多年生落叶丛生小灌木。它的根、干、皮、叶及果实中均含对某些昆虫有毒杀作用的化学成分[1 5]。我们用活性跟踪法以金龟甲,菜青虫为试虫跟踪分离提取,从紫穗槐叶的乙醇提取物中分离出对金龟甲、菜青虫等有毒杀作用的混合物。经层析分离得到5个化合物纯品。用波谱等方法鉴定为:6α,12α 脱氢 鱼藤素;6α,12α 脱氢 α 灰叶酚;(±) 灰叶素;( ) 6 羟基 6α,12α 脱氢 灰叶酚;鱼藤酮。1　实验部分1 1　仪器与试剂X 4型显微熔点仪(温度计未校正);三用紫外分析仪;布鲁克EQUINOX 55…     

α-羟基取代膦酸酯类化合物的合成研究进展

含磷化合物一直是有机化学研究的热点之一,许多合成药物以及天然产物都含有磷原子。其中,α-羟基取代膦酸酯类化合物是重要的有机合成中间体,其在有机合成中的应用一直受到广泛关注。文章详细综述了α-羟基取代膦酸酯类化合物的合成方法。     

Pd/C催化氧气对1,3-二羰基化合物的α-位氧化

以碳酸钾作碱,DMF作溶剂,5%Pd/C催化1,3-二羰基化合物在室温下与氧气反应,直接得到α-羟基化合物,其结构经NMR和MS表征.     

一种新型钛调整体系——钛羰酸盐和锂试剂的还原反应

本文首次将一系列α-芳香族酮酸通过与钛酸醉酯[Ti(OR~1)_4]的交换反应制备成钛羧酸盐,随后将它与锂试剂反应.在此体系中锂试剂发生了一个未见报道的新反应:将α-芳香族酮酸还原为相应的α-羟基羧酸.进一步研究表明,锂试剂同时可以发生加成反应,且因Ti(OR~1)_4,酮酸和锂试剂的不同,加成与还原的比例也随之不同.     

6-羟基染料木素与8-羟基染料木素的制备及生物活性研究进展

6-羟基染料木素(6-OHG)和8-羟基染料木素(8-OHG)是染料木素A环上C6或C8位发生羟基化反应生成的衍生物,其分子中有更多酚羟基,同时含有邻二酚羟基结构,这也使它们的生物活性与染料木素相比发生了显著变化。研究表明,6-OHG和8-OHG具有抗氧化、抗诱变、抑制磷酸二酯酶3B活性、抗糖化、保肝、抗黑色素生成作用、改善记忆力等广泛的药理活性。本文将对6-OHG和8-OHG的来源、制备方法和生物活性研究进行综述,以期为两个化合物的开发利用提供参考。     

乙酰衍生化气相色谱-电子捕获检测法分析尿中α-羟基三唑仑和α-羟基阿普唑仑

三唑仑和阿普唑仑是目前国内麻醉抢劫案件中最常使用的两种麻醉药物。为确定案件性质及取得证据等原因,案件发生后常需要进行受害人血、尿等体液中药物或其代谢物的分析。这两种药物作用强、剂量小,服药后血中药物及其代谢物的浓度都很低,尿中药物的浓度也很低。相对而言,尿中代谢物α-羟基三唑仑(α-hydroxytrizolam,简写为α-     

β-(3,4-二羟基苯基)-α-羟基丙酸异丙酯/冰片酯合成研究

以3,4-二羟基苯甲醛为起始原料, 经苄基保护、Darzens环氧化、Lewis酸开环、NaBH4还原、催化加氢脱保护得到β-(3,4-二羟基苯基)-α-羟基丙酸异丙酯和β-(3,4-二羟基苯基)-α-羟基丙酸冰片酯, 所得化合物的结构通过1H NMR、13C NMR, IR, MS证实. 该方法操作简单、毒性低、产物易于纯化.     

胶束毛细管电动色谱法用于祖师麻中5种主要成分的测定

采用胶束毛细管电动色谱法分离和测定祖师麻中紫丁香苷(SR)、7-甲氧基香豆素(7-MC)、瑞香苷(DN)、瑞香素(DP)和7-羟基香豆素(7-HC)等5种组分,通过研究影响分离和测定的主要因素,建立一种快捷、简便的方法用于5种组分的分离测定.在最佳电泳介质(10 mmol/L SDS pH=9.0,20 mmol/L硼酸盐缓冲溶液)中,5种待测组分在8 min内实现基线分离.SR、7-MC、DN、DP和7-HC的线性响应范围分别为1.0~100、1.5~100、5.0~75、5.0~75和1.0~75!g/mL;检测限分别为0.3、0.5、1.7、1.7和0.3!g/mL.方法成功应用于实际样品祖师麻注射液及祖师麻片中SR、7-MC、DN、DP和7-HC的含量测定.     

藏药蕨麻多糖水解单糖的毛细管区带电泳分离研究

以1-萘基-3-甲基-5-吡唑啉酮(NMP)为柱前衍生试剂,探讨了毛细管区带电泳模式下对藏药蕨麻多糖水解液中单糖的分离条件。实验采用58.5 cm×50μm i.d.毛细管(有效长度50 cm),55 mmol/L硼酸盐缓冲溶液(pH=9.46),柱温20℃,分离电压22 kV,进样10 s。该法不加任何添加剂,9种单糖可高效、快速基线分离,实现了对藏药蕨麻多糖水解液中单糖的分离和定量分析,结果令人满意。     

Lithium Perchlorate Diethyl Ether Solution: A Highly Efficient Media for the Abramov Reaction

The f -hydroxy phosphonates are readily prepared by treating aromatic or aliphatic aldehydes and ketones with trialkylphosphite in the presence of trimethylsilylchloride in a very short time and in almost quantitative yields.     

Crystal Structure of O，O－Diethyl－α－（β－triphenylgermanyl）－propionoyloxy Methylphosphonate

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＯ，Ｏ－Ｄｉｅｔｈｙｌ－α－（β－ｔｒｉｐｈｅｎｙｌｇｅｒｍａｎｙｌ）－ｐｒｏｐｉｏｎｏｙｌｏｘｙＭｅｔｈｙｌｐｈｏｓｐｈｏｎａｔｅＣｈｅｎＲｕ－Ｙｕ；ＭａｏＬｉ－Ｊｕａｎ；ＬｉｕＡｉ－Ｌｉｎ（Ｉｎｓｔｉｔｕｔｅｏ...     

Synthesis of 2-(α-Hydroxyalkyl)-2-Oxazoline under Microwave Irradiation in Bluk

Four 2-(α-hydroxyalkyl)-2-oxazolines and a 2-(α-hydroxy-α,α-diphenyl)-2-benzooxazole were synthesized from β-amimoalcohols and α-hydroxy carboxylic acids under microwave irradiation in the absence of a solvent.     

New Chemistry of Enol Phosphates

Applications of enol phosphates in the synthesis of novel bicyclic 1,3-dienes, bi- and polycyclic aromatic derivatives, and f -hydroxy ketones are described.     

碘小姐的旅行

将碘元素拟人化,让其以卤素家族四小姐的身份,在这美丽的世界上走一走,并拟人化讨论了碘小姐的元素分布、物理性质以及生理活性,让读者在获得知识之余还能有美的享受。     

Extraction and simultaneous determination of metoprolol and α-hydroxy metoprolol in latent fingerprints by liquid chromatography tandem mass spectrometry

Abstract

A simple extraction and sensitive simultaneous analysis method for metoprolol and its metabolite alpha-hydroxy metoprolol in latent fingerprint using liquid chromatography-mass spectrometry was developed. The extraction procedure was optimized as scrubbing using cotton swabs for 30 times followed by ultrasonic assistance in 30?°C methanol for 5?min with power of 2000 W. Drug analysis was performed using the mixture of methanol and 0.1% formic acid solution (pH 3.5, 30:70, v/v) as the mobile phase under positive electrospray ionization condition. The linear range obtained was 1.0–500.0?ng/mL for MET, and α-MET, and the limit of detection and the limit of quantification were 0.3?ng/cotton swab and 1.0?ng/cotton swab, respectively. The method showed very slight matrix effect and good recovery to the analytes in the fingermarks. Evaluation of extraction substrates and developing methods showed that the method developed is best used for impermeable substrates and that the commercially development powders have very slight influence on the qualitative detection of metoprolol in fingermarks. Finally, the drug users distinguishing test proved that the method developed for pharmaceuticals could be applied in the forensic analysis for circling out the pool of suspects in the criminal investigation based on their drug use history.     

Thermodynamic functions of α,α-trehalose dihydrate and of α,β-trehalose monohydrate at temperatures from 13 K to 300 K

Thermodynamic properties at low temperatures were investigated for α,α-trehalose dihydrate and α,β-trehalose monohydrate. The heat capacities were measured using an adiabatic calorimeter at temperatures between 13 K and 300 K. The heat capacity data were expressed as a function of temperature, T, by a polynominal of forth to sixth order, with which thermodynamic functions, enthalpy, entropy, and Gibbs free energy, were determined.     

Fermented Baker's Yeast: An Efficient Catalyst for the Synthesis of Pyran Derivatives in Water at Room Temperature

An environmentally friendly, one-pot synthesis of biologically important pyran derivatives in water is described herein. The advantages of this method are its simplicity, cost-effectiveness, and environmental friendliness. Water was exploited both as reaction media as well as activator of catalyst (fermentation of bakers' yeast). Compared with other methods for synthesis of pyran derivatives, satisfactory results were obtained with good yields under simple experimental procedure.     

Expedient synthesis of pyrazoles substituted with amino, hydroxyl and thioamide groups

The reaction of α,β-acetylenic γ-hydroxy nitriles with thiosemicarbazide, under mild conditions (rt, no catalyst, in 1:1 aqueous ethanol, 4-14 h), proceeds chemo-, regio- and stereoselectively to give atypically so far inaccessible tri-functionalized (amino, hydroxyl and thioamide groups) pyrazoles in 53-91% yields. The hydroxyl function is easily protected by using the corresponding acetals of the starting acetylenic hydroxy nitriles.