气相色谱-质谱联用法测定维生素C泡腾片中的甜蜜素

采用气相色谱-质谱(GC-MS)选择离子监测法(SIM),建立了准确可靠、灵敏度高、快速简便的测定维生素C泡腾片中甜蜜素含量的新方法.样品中的甜蜜素衍生后用有机试剂提取,在选择离子模式下进行测定,以保留时间和特征离子比例进行定性,单离子定量.甜蜜素的线性范围为0.05-10mg/L,检出限为0.6mg/kg,回收率为90.5%-96.9%,相对标准偏差小于4.4%.方法分析所用时间短,结果准确可靠,选择性好,适用于维生素C泡腾片中甜蜜素含量的检验.     

环境光对谷氨酸钠溶液近红外激光拉曼光谱的影响

探讨了环境光,对谷氨酸钠溶液的近红外激光拉曼光谱的影响。研究表明不同的环境光,自然光和室内荧光灯光,均会对近红外拉曼光谱产生不同的干扰效应,存在着特征谱峰,倒峰或尖锐正峰。虽干扰表现不同,但都有影响,不能忽略。建议在进行溶液近红外激光拉曼光谱检测时,须在暗室或暗罩中进行,以完全隔离环境光的影响。     

显微-反射傅里叶变换红外光谱研究油酸钠与胶磷矿吸附机理

红外光谱已经成为浮选药剂作用机理研究的最重要手段之一。由于矿物本身具有较强的红外吸收,传统溴化钾压片透射光谱很难检测到矿物表面吸附药剂的微弱红外信号。采用显微-傅里叶变换红外光谱仪的反射模式,测定了不同浓度油酸钠在胶磷矿表面的吸附形式,并观察了吸附形貌。结果表明,与透射红外光谱相比,反射红外光谱对表面有更高的灵敏度,能更好地揭示实际浮选药剂浓度下的吸附机理。碱性条件下当油酸钠浓度较低时,油酸离子与表面晶格钙离子发生化学吸附,吸收峰在1 552 cm-1,同时也存在油酸钙沉淀的物理吸附,吸收峰在1 570和1 535 cm-1;当油酸钠浓度超过临界胶束浓度时,胶束使得胶磷矿表面亲水,导致油酸钠溶液残留在表面,吸收峰在1 560 cm-1,掩盖了其他吸收峰;表面经水洗涤后药剂吸收峰强度大幅减弱,是由于残留的油酸钠和物理吸附的油酸钙被洗掉。另外,随着油酸钠浓度增大,药剂二维形貌由点状吸附聚集为片状吸附,覆盖面积增大,但并不是完全覆盖,这与矿物表面异质性有关。以上研究结果有利于理解磷矿石提磷或铁矿石脱磷浮选体系中捕收剂与胶磷矿的作用机理。     

基于FTIR技术的酸牛奶营养成分快速检测方法研究

酸牛奶作为一种重要的发酵乳制品,伴随着发酵过程,其各种营养成分时刻发生着复杂的变化,因此,建立酸牛奶的快速高效检测技术可以实现对生产过程的实时监控,这也是食品安全监管要达到的重要目标。傅里叶变换红外光谱技术(FTIR)因其快速、高通量、无化学污染、可对掺假成分予以分辨等特点被广泛应用于食品安全领域。以FTIR技术为核心,利用氟化钙薄膜法,将酸牛奶FTIR光谱图与其营养成分(能量值,蛋白质、脂肪、碳水化合物和钠含量)对照,建立了基于最小二乘法(PLS)的定量化预测模型。结果表明,该模型样品校正集的能量值,蛋白质、脂肪、碳水化合物和钠含量的交叉检验R2值分别达到0.938 9,0.926 6,0.918 6,0.941 8和0.977 1;该模型用于预测,其样品验证集的交叉检验R2值分别为0.920 5,0.905 3,0.908 5,0.939 3和0.936 4。由此可见,该模型对酸牛奶各营养指标均具有较好的预测准确性,在时间上具备较好的稳定性。不同于传统的化学检测方法,本研究为实现对酸牛奶品质的快速检测提供了一种较为可行的方法。该方法作为乳制品质量监控技术的一项初步探索,具有较好的应用前景。     

The collagen type I segment long spacing (SLS) and fibrillar forms: Formation by ATP and sulphonated diazo dyes

The collagen type I segment long spacing (SLS) crystallite is a well-ordered rod-like molecular aggregate, ∼300 nm in length, which is produced in vitro under mildly acidic conditions (pH 2.5–3.5) in the presence of 1 mM ATP. The formation of the SLS crystallite amplifies the inherent linear structural features of individual collagen heterotrimers, due to the punctate linear distribution and summation of the bulkier amino acid side chains along the length of individual collagen heterotrimers. This can be correlated structurally with the 67 nm D-banded collagen fibril that is found in vivo, and formed in vitro. Although first described many years ago, the range of conditions required for ATP-induced SLS crystallite formation from acid-soluble collagen have not been explored extensively. Consequently, we have addressed biochemical parameters such as the ATP concentration, pH, speed of formation and stability so as to provide a more complete structural understanding of the SLS crystallite. Treatment of collagen type I with 1 mM ATP at neutral and higher pH (6.0–9.0) also induced the formation of D-banded fibrils. Contrary to previous studies, we have shown that the polysulphonated diazo dyes Direct red (Sirius red) and Evans blue, but not Congo red and Methyl blue, can also induce the formation of SLS-like aggregates of collagen, but under markedly different ionic conditions to those employed in the presence of ATP. Specifically, pre-formed D-banded collagen fibrils, prepared in a higher than the usual physiological NaCl concentration (e.g. 500 mM NaCl, 20 mM Tris-HCl pH7.4 or x3 PBS), readily form SLS aggregates when treated with 0.1 mM Direct red and Evans blue, but this did not occur at lower NaCl concentrations. These new data are discussed in relation to the anion (Cl⁻) and polyanion (phosphate and sulphonate) binding by the collagen heterotrimer and their likely role in collagen fibrillogenesis and SLS formation.     

标准加入ICP-AES法测定铬酸钠中杂质元素

采用ICP-AES法同时测定工业铬酸钠溶液中微量Al,Ca,Fe,Mg,Si杂质元素。针对测定过程中存在的基体干扰、谱线干扰等问题,通过实验确定了铬酸钠中微量的Al,Ca,Fe,Mg,Si的分析测试谱线:Al 167.079nm,Ca 393.366nm,Fe 259.940nm,Mg 279.533nm,Si 251.61nm。实验用优级纯HCl将待测溶液调为酸性,消除工业铬酸钠溶液酸度不稳定引起的测定误差,采用标准加入法消除基体干扰,探讨了Al,Ca,Fe,Mg,Si等五种微量组分检测方法标准曲线线性相关性、检出限、精密度以及回收率等分析指标,详细研究了在选定分析谱线下,标准加入法对铬酸钠溶液中Al,Ca,Fe,Mg,Si等微量杂质含量测定结果的准确性的影响。结果表明标准曲线呈线性关系(R2=0.998 8~0.999 6之间),五种元素检出限在(0.013 4~0.028 0)mg·L-1之间,11次测量标准偏差小于5.86%,回收率在97.30%~107.50%之间。实验建立的分析方法的检出限、精密度、准确度均能满足分析测试要求;方法实用性强,已经成功用于离子膜电解法中铬酸钠原料液微量离子检测;利用铬酸钠、重铬酸钠和重铬酸酐与溶液酸度的关系,实验建立的分析方法还可拓展于重铬酸钠及铬酐甚至其他六价铬产品中Al,Ca,Fe,Mg,Si杂质离子的检测,同时也可以扩展到上述样品中其他杂质元素的测定。     

Up-regulation of Na expression in the area postrema of total sleep deprived rats by TOF-SIMS analysis

Area postrema (AP) is a circumventricular organ plays an important role in sodium homeostasis and cardiovascular regulation. Since sleep deficiency will cause cardiovascular dysfunction, the present study aims to determine whether sodium level would significantly alter in AP following total sleep deprivation (TSD). Sodium level was investigated in vivo by time-of-flight secondary ion mass spectrometry (TOF-SIMS). Clinical manifestation of cardiovascular function was demonstrated by mean arterial pressure (MAP) values. Results indicated that in normal rats, TOF-SIMS spectrum revealed a major peak of sodium ion counting as 5.61 × 10⁵ at m/z 23. The sodium ions were homogeneous distributed in AP without specific localization. However, following TSD, the sodium intensity was relatively increased (6.73 × 10⁵) and the signal for sodium image was strongly expressed throughout AP with definite spatial distribution. MAP of TSD rats is 138 ± 5 mmHg, which is significantly higher than that of normal ones (121 ± 3 mmHg). Regarding AP is an important area for sodium sensation and development of hypernatremic related sympatho-excitation; up-regulation of sodium expression following TSD suggests that high sodium level might over-activate AP, through complex neuronal networks involving in sympathetic regulation, which could lead to the formation of TSD relevant cardiovascular diseases.     

(S)-1-苄基-3-羟基吡咯烷的合成及红外光谱研究

从L-苹果酸出发,经过与苄胺缩合反应得到(S)-1-苄基-3-羟基吡咯烷-2,5-二酮,再通过硼氢化钠-碘体系还原制得重要的医药中间体(S)-1-苄基-3-羟基吡咯烷。采用红外光谱法对原料、中间体及产物进行了测试并对硼氢化钠-碘体系还原酰亚胺的机理进行了研究。通过比较原料、中间体及产物相应特征吸收峰的消失或是出现,可知所得的产物为(S)-1-苄基-3-羟基吡咯烷;还原机理研究表明,硼氢化钠在碘催化下生成的硼烷与酰亚胺中的羰基形成四元环状过渡态,同时另外一分子硼烷与酰亚胺中的氮原子形成N-BH3复合物,然后羰基还原完全,得到(S)-1-苄基-3-羟基吡咯烷-硼烷复合物,最后在甲醇作用下脱去硼烷得到最终产物。     

茜素分光光度法测定磷霉素钠

在乙醇体系中,磷霉素钠与茜素发生反应,生成稳定的1∶1的络合物,溶液颜色发生明显改变,其最大吸收波长为545nm,磷霉素钠的浓度在1.4—60mg·L-1范围内遵守比耳定律,表观摩尔吸光系数ε=3.47×103L·mol-1.cm-1,基于以上反应,本方法测定药物制剂含量与文献方法一致,回收率在99.6%—100.5%之间,结果满意。     

原子吸收光谱法和ICP-AES测定水中钠的比较

测定水中钠的含量,ICP-AES具有直接进样、测量稳定、校准曲线线性范围宽等特点;而原子吸收光谱法需要加入消电离剂硝酸铯或氯化铯,实际操作麻烦.该方法经过t检验证明与标准方法无显著性差异,加标回收率为96.9%-104%,可以代替原子吸收光谱法,相对标准偏差各为0.7%、0.8%.