水解-Cu(Ⅱ)沉淀间接原子吸收法测定头孢氨苄

基于在pH4.0～5.4醋酸钠介质中,头孢氨苄于100℃下的水解产物能定量与Cu（Ⅱ）作用生成沉淀,测定反应后剩余的Cu（Ⅱ）,可间接测定头孢氨苄.方法操作简便,重现性好,线性范围5～300 mg/L,回收率为98%～105%.测定结果与药典法比较基本一致.     

山苍子油毛细管气相色谱分离及成分的色/质谱鉴定

首次采用毛细管色谱及色/质联用技术对云南山苍子油进行分离及成分直接定性,并提出了对其主成分柠檬醛的一种恒温毛细管色谱定量方法。     

Preparation of the selenomethionine derivative of tabtoxin resistance protein

In order to obtain phase information for the X-ray diffraction of tabtoxin resistance protein (TTR) crystal using the MAD phasing method, a selenomethionine (Se-Met) derivative of TTR was overexpressed in E. coli strain M15, with pQE-30 plasmid, through IPTG induction in M9 medium containing Se-Met. The product was purified to an estimated homogeneity of greater than 95% according to SDS-PAGE, by a Ni-NTA metal affinity followed by a Mono Q anion exchange column chromatography. The successful substitution of Se-Met for methionine (Met) was confirmed by MALDI-TOF and ESI-Quadrupole Mass Spectrometry analysis. The derivative crystal was obtained using similar conditions as those for the native.     

高纯氯化铯中锂,钠,钾,铷的测定

采用火焰原子吸收法测定了氯化格中锂、钠、钾、铷的含量,测定灵敏度高,回收率９５％～１０６％,相对偏差低于 ７．８％．方法简便快捷．     

HS-SPME/GC-MS/GC-O对镇江香醋特征香气成分的确定

采用顶空固相微萃取提取了镇江香醋的挥发性成分,用气相色谱-质谱联用技术结合气相色谱-嗅觉测量法以及化合物的保留指数,鉴定了镇江香醋的主要香气成分;同时利用气相色谱-嗅觉测量技术,采用探测频率和探测强度相结合的办法,初步确定了乙酸、3-甲基丁酸、乙酸乙酯、乙酸-3-甲基-丁酯、乙酸苯乙酯、苯乙醇、2,3-丁二酮、二氢-5-戊基-2(3H)-呋喃酮、2-甲基丙醛、3-甲基丁醛、糠醛、苯甲醛、三甲基恶唑、2,3-二甲基吡嗪、三甲基吡嗪、四甲基吡嗪16种化合物为镇江香醋的特征香味物质.     

β-环糊精交联树脂富集氢化物发生-原子荧光光谱法测定水样中的苯基汞

提出利用β-环糊精交联聚合树脂富集环境水样中的苯基汞,选用乙醇洗脱富集的苯基汞,并使用氢化物发生-原子荧光光谱法对其消解物进行定量分析的方法,通过实验优化其化学和仪器条件。讨论了溴化剂用量、溴化时间对消解率的影响,振荡时间对吸附率的影响,洗脱时间对洗脱率的影响,以及共存离子干扰、精密度与检出限等因素,对样品进行了分析并绘制了标准曲线。该方法灵敏度高、选择性好、精密度高,检出限为0.36 ng/mL,相对标准偏差RSD为2.29%(n=10,c=4 ng/mL)。     

固相萃取-气相色谱/质谱法测定河水中16种多环芳烃

建立了固相萃取-气相色谱/质谱联用测定河水中16种多环芳烃(PAHs)的分析方法。结果表明,以C18为固相萃取柱、10 mL正己烷为洗脱剂,在上样速率为5 mL/min的条件下,用于河水中16种PAHs的检测,均有较好的回收率,在1～200μg/L范围内呈良好的线性关系,相关系数在0.999 46～0.999 99之间,检出限为0.002 6～0.081 3μg/L,加标回收率为91%-119%,相对标准偏差(RSD)在2.4%～9.2%(n=6)之间。方法简便可靠,能够达到水样中16种多环芳烃的检测要求。     

分光光度法测定饮料中的碘

本文利用碘-淀粉蓝色络合物在λ=580nm具有强吸收特性,用干灰化法处理饮料样品,以分光光度法测定饮料中微量碘,方法的特点是高灵敏度(ε=7.86×104 L mol-1cm-1)、高精密度、线性范围适宜(0～2.0g/ml)相关性好(相关系数r=0.9996)、方法简便易行等,可广泛应用于饮料中碘含量的测定。     

Sequencing of phosphopeptides sulfonated by 4-sulfophenyl isothiocyanate using post-source decay matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

Phosphorylation/dephosphorylation is probably the most common and important reversible post-translational modification of proteins. Analyzing the functional effects of phosphorylation is helpful for understanding the biological functions of proteins. Identification of the phosphorylation sites of phosphorylated protein is a prerequisite for research on phosphorylation. In this work, an effective and simple method of identification of protein phosphorylation sites has been developed. Phosphopeptides were selectively enriched with immobilized metal affinity chromatography (IMAC) and subsequently chemically modified by 4-sulfophenyl isothiocyanate, and then the chemically modified phosphopeptides were sequenced with post-source decay (PSD) matrix-assisted laser desorption/ionization (MALDI) time-of-flight mass spectrometry for detecting phosphorylation sites. The charge of derivatization by 4-sulfophenyl isothiocyanate introduces a negative sulfonic acid group at the N-terminus of a peptide, and enables the selective detection of only a single series of C-terminal y-type ions. This chemically assisted method greatly simplifies the extremely complex pattern of PSD fragment ions and makes the PSD spectra more easier to be interpreted. The phosphorylation sites of a synthesized model phosphopeptide and human c-myc protein have been successfully identified by this method.