对某医药-护肤液成分的剖析研究

采用了溶剂抽提与多种仪器相配合的分析方法，对某医药-护肤液的成分进行了剖析．其主要医药成分的富集，以乙醚为最佳，浓缩富集物的纯度可达99％．以高效液相色谱(HPLC)、质谱(MS)、红外光谱(IR)、元素分析等几种仪器分析相互配合完成了样品的定性、定量测定．结果表明，此护肤液的主要医药成分为氯霉素(D(-)threo-2，2-dichloro-N-[β-hydroxy-α-hydroxymethyl)-P-nitrophenethyl)acetamide，chloramphenicol，chloromycetin)．主要美容基质成分为1，2-丙二醇．此外，还有罗红霉素、地塞米松、乙二醇、乙醇等成分．     

北苍术超临界CO2萃取产物的成分

用气相色谱－质谱－计算机联用法分析了北苍术的超临界CO2萃取产物的成分,鉴定出苍术酮、β－桉叶油醇、苍术醇31化合物,占出峰总面积的88．1％,并与传统水蒸汽蒸馏法（SD）提取的挥发油成分进行了对比。结果证明,两种方法抽提的苍术主成分基本相同,但超临界CO2萃取产物比SD产物多出现了一些重质组分,萃取更完全而有效。     

香椿子油成分的 GC-MS分析

用正己烷抽提得香棒子,然后将样品进行皂化、甲酯化,以毛细管色谱－质谱联用法（GC－MS）测定了香棒子油的组成,共鉴定出39种成分,其中亚油酸相对含量为83．45％。     

低碳醇合成Raney Cu－Co催化剂的研究Ⅱ．Cu－Co－Al合金及Raney Cu－Co催化剂的XRD表征

本文对Ｃｕ／Ｃｏ比不同的五个Ｃｕ－Ｃｏ－Ａｌ合金样及其碱抽提产物──ＲａｎｅｙＣｕ－Ｃｏ催化剂的体相结构进行了ＸＲＤ表征。结果表明：Ｃｕ－Ｃｏ－Ａｌ合金由ＣｕＡｌ、ＣｕＡｌ＿２及Ａｌ＿（１３）Ｃｏ＿４三种物相构成。随Ｃｕ／Ｃｏ原子比（０．１７～２３．１）增高，Ａｌ＿（１３）Ｃｏ＿４及ＣｕＡｌ物相逐渐减少，直至消失，ＣｕＡｌ＿２物相产生且逐渐增多。ＲａｎｅｙＣｕ－Ｃｏ催化剂由两种Ｃｕ－Ｃｏ固溶体组成，一种富铜，另一种富钴。Ｃｕ－Ｃｏ固溶体的形成发生于碱抽提或还原过程，含钴物相的存在有利于ＣｕＡ１物相的碱抽提。     

高效液相色谱法测定橡胶促进剂TBBS

采用反相高效液相色谱法（HPLC）测定了橡胶促进剂N－叔丁基－2－苯并噻唑次磺酰胺（TBBS）的纯度，标准偏差小于0．3。     

(E)-4,4′-二氨基二苯乙烯-2,2′-二磺酸的反相高效液相色谱法

1引言（E）－4，4’一二氨基二苯乙烯一2．2’一二磺酸［（E）－DASj是合成染料和荧光增白剂的重要中间体，它由对硝基甲苯邻磷酸空气氧化、铁粉还原、碱液中和与酸析得到，样品含量一般为92％～96％。现常用化学法和紫外光度法分析。作者曾建立离子对HPLC法，同时分离了样品中4种中间副产物，但分离时间较长（3min）。本文建立反相HPLC法，具有简便快速、灵敏度高、选择性好的特点。2实验部分2．1仪器与试剂Shimadzul。C－6A型高效液格色谱仪。PELambda17型紫外可见分光光度计。Millipore超纯水仪。ShimadzuAA－67O原子吸收分光…     

栾树种油中脂肪酸组成的气相色谱-质谱分析

用乙醚抽提栾树种油,将样品皂化和甲酯化后,用毛细管质谱－色谱法（ＧＣ－ＭＳ）测定了栾树种油的脂肪酸组成,共鉴定出２１种成分,其不饱和脂肪酸相对含量为８８％,主要成分为二十碳烯酸和亚油酸,安们的相对含量分别为４４．９８％和３９．７５％。     

（E）－2－甲基－1，3－戊二烯的振动光谱及其稳定构象的研究

记录了（Ｅ）－２－二甲基－１，３－戊二烯的固、液、气态ＦＴＩＲ光谱（４００～４０００ｃｍ~（－１））和固、液态Ｒａｍａｎ光谱（５０～４０００ｃｍ~（－１）），观测了６８５及６５８ｃｍ~（－１）谱线的变温ＦＴＩＲ光谱（－７３～１０℃）．对所得谱图进行的指认分析发现，该化合物存在两种单键旋转构象异构体ｓ－ｔｒａｎｓ和ｓ－ｃｉｓ，由变温ＦＴＩＲ光谱峰强度随温度的变化得到这两种构象互变的ΔＨ~０和ΔＳ~０。     

石墨化碳黑净化柱结合HPLC－PDA和LC－MS/MS快速检测苹果汁中展青霉素

基于石墨化碳黑材料制备了一种固相萃取柱（GCB柱）,结合高效液相色谱－二极管阵列检测法（HPLC－PDA）和液相色谱－串联质谱法（LC－MS/MS）评估了GCB柱和4种商业化固相萃取柱（Retain AX、PAX、MAX和HLB）的净化效果,并对澄清型苹果汁中影响展青霉素准确定量的杂质进行了分析。结果发现,苹果汁经上述5种净化柱净化后,大大降低了杂质干扰,色谱图、信噪比和基质效应显著改善。其中,GCB净化为HPLC－PDA分析提供了理想的色谱图,为LC－MS/MS分析提供了可接受的基质效应（-14%）、优于HLB净化的色谱图以及与Retain AX净化相当的信噪比。建立的稳定同位素稀释－液相色谱－串联质谱法（SIDA－LC－MS/MS）可以克服基质效应和净化损失对检测结果准确性的影响。采用HPLC－PDA和SIDA－LC－MS/MS分析时,GCB净化比HLB净化的方法更灵敏;MAX、HLB和GCB净化均能得到较好的回收率（82% ~ 102%）和较小的相对标准偏差（≤ 9%）。所开发的GCB净化方法仅需上样和洗脱2步,且在重力作用下过柱仅需10 min,比其他固相萃取净化更简单快捷,净化能力良好。实际样品经GCB柱净化和HPLC－PDA、SIDA－LC－MS/MS分别分析,展青霉素的平均含量为34 μg·kg-1。GCB柱较好的净化效果和较低的使用成本将有助于其在展青霉素常规检测中的广泛应用。     

铁（Ⅲ）－柠檬酸水溶液中的离子平衡

铁（Ⅲ）－柠檬酸水溶液中的离子平衡李定（中南工业大学子弟中学长沙４１００８３）关键词铁（Ⅲ）－柠檬酸水溶液，离子平衡，浓度－ｐＨ图铁（Ⅲ）和柠檬酸是许多食品和饮料的重要成分，也是血液中的成分之一。据报道￣［１］，在血浆中含有大约０．１ｍｏｌ·ｄｍ￣（...     

蓝色圆珠笔字迹的高效液相色谱分析与模式识别研究

该文收集市售蓝色圆珠笔样品16份,结合模式识别技术对其高效液相色谱数据进行研究。利用相关系数法计算色谱图相对峰面积的相似度,定量地评价样品间的差异性。选取16个样品3个批次间的最小相似度(λ=0.92)作为判定是否源于同种样品的阈值,相似度小于0.92的数据为89份,占全部比对样品的74.2%;根据液相色谱图的保留时间、峰数及峰形差异将所有样品分为3类,进一步利用系统聚类法依据相似度的大小将第一类样品分为3小类。该文提出的采用相对峰面积相似度评价样品差异的方法,能够显著提高分辨能力,促进圆珠笔字迹的自动化识别。高效液相色谱法获取数据,模式识别技术分析数据的方法为圆珠笔字迹的分类与鉴别提供了新思路。     

运用色谱指纹图谱与化学计量学方法对灵芝进行分类

采用95%乙醇为提取溶剂,运用高效液相色谱(HPLC)指纹图谱技术与化学计量学方法,对11个不同灵芝菌株子实体进行分类。通过相似度分析分别获得提取样品指纹图谱的13个共有峰及每个样品之间的相似度;以相对共有峰面积为分析参数,运用化学计量学方法包括聚类分析(HCA)、主成分分析(PCA)及判别分析(DA)对其进行分类,结果分为紫芝、赤芝和美国大灵芝3类。实验结果表明,用化学计量学的方法对灵芝样品的指纹图谱数据进行分析,是一种可用于其分类的科学方法。     

香港海域毒性微藻Alexandium tamarense的麻痹性贝毒研究

对从香港海域底坭分离并培养的毒性微藻塔玛亚历山大藻（Alexandiumtamareuse）的毒性和麻痹性贝毒素的组成进行研究。由生物试验测得其毒性为4．11×10－6MU／cell，用高效液相色谱分析毒素的组成，结果表明所含麻痹性贝毒成分主要是膝沟藻毒素－2（GTX2），含量为94.13pg／cell，本研究所用的微藻毒素提取方法和高效液相色谱分析方法都比较容易和有效。     

Simultaneous Determination of Quercetin and Luteolin in Dried Flowers by Multivariate HPLC-ECD Calibration

Two calibration models, partial least squares (PLS) and principal component regression (PCR), were applied to the simultaneous determination of quercetin and luteolin by high performance liquid chromatography (HPLC) with electrochemical detection (ECD). The proposed methods were successfully applied to the analysis of dried flower samples. It was found that the relative standard errors of prediction (RSEP) for the validation set of PLS of quercetin and luteolin was 1.31 and 2.23%, and the RSEP of PCR was found to be 3.56 and 4.32%, respectively. Several dried flower samples were analysed and the recoveries were in the range of 95.9–103.3%.     

水样中氟罗沙星和磺胺喹噁啉的离子液体均匀提取

提出一种新的离子液体均匀提取方法,即向水样中加入可溶于水的离子液体1-己基-3-甲基咪唑四氟硼酸盐([C6MimBF4]),再加入过量六氟磷酸铵(NH4PF6),形成不溶于水的离子液体1-己基-3-甲基咪唑六氟磷酸盐([C6MimPF6]),水样中的氟罗沙星和磺胺喹噁啉被提取到[C6MimPF6]相,离心分离后,离子液体可直接用于HPLC分析.本法测得的氟罗沙星和磺胺喹噁啉的检出限分别为1.8和1.1μg/L.     

Investigation of the limitations of saturated fractional factorial experimental designs,with confounding effects for an HPLC ruggedness test

Summary Recently much attention has been directed to the validation of analytical methods. The level of validation will depend on the method application. If a method is developed for general use, for instance by different analysts, instruments or laboratories, then the effect of these changes need evaluation. This is normally referred to as ruggedness testing, where the limitations of the method to changes in the specified conditions are examined.This paper examines the use of Plackett-Burman fractional factorial experiment designs for ruggedness testing in high performance liquid chromatography (HPLC). The ability of these designs to identify confounding effects is applied to the stability indicating analysis of Salbutamol and its major degradation product, AH4045. The results show that confounding effects, proving extremely pertinent to HPLC, can be identified.The assay proved rugged to most tested changes although not to the use of column packing material from different manufacturers.     

Determination of Plant Thiols by Liquid Chromatography Coupled with Coulometric and Amperometric Detection in Lettuce Treated by Lead(II) Ions

The main aim of this paper is to utilize high performance liquid chromatography with electrochemical detection for determination of thiols content in plants tissues of lettuce treated with lead(II) ions (0, 0.5 and 1 mM). We used two HPLC‐ED instruments: HPLC coupled with one channel amperometric detector and HPLC coupled with twelve channel coulometric detector to detect simultaneously twelve thiols. The detection limits of thiols measured by CoulArray detector were about two magnitudes lower in comparison to those measured by Coulochem III detector and were from tens to hundreds pM. Under the optimal conditions, we utilized HPLC‐CoulArray detector for analysis of tissues from lettuce plants. In addition, distribution and accumulation of lead ions with high spatial resolution was monitored using laser induced breakdown spectroscopy.     

Dispersive Liquid‐Liquid Microextraction Followed by HPLC‐DAD as an Efficient and Sensitive Technique for the Determination of Patulin from Apple Juice and Concentrate Samples

A simple and sensitive method based on dispersive liquid‐liquid microextraction (DLLME) in conjunction with high performance liquid chromatography‐diode array detection (HPLC‐DAD) has been developed for the quantitative analysis of patulin in apple juice and concentrate samples. The effect of extraction and disperser solvent (nature and volume), pH of sample solution, extraction time and extraction temperature was investigated. Under the optimal conditions the linear dynamic range of patulin was from 8.0 to 40.0 μg L^‐1 with a correlation coefficient of 0.9993 and a detection limit of 4.0 μg L^‐1. The relative standard deviation (RSD) was less than 5.9% (n = 5) and the recovery values were in the range of 94‐97%. Finally the proposed method was successfully applied for the analysis of patulin in apple juice and concentrate samples.     

杜仲中京尼平甙酸的硅胶柱色谱分离纯化及反相高效液相色谱/液相色谱-电喷雾质谱/核磁共振鉴定

 建立了杜仲中京尼平甙酸的硅胶柱色谱分离纯化及反相高效液相色谱/液相色谱-电喷雾质谱/核磁共振(RP-HPLC/LC-ESI-MS/NMR)鉴定方法。杜仲皮经粉碎后,用70%乙醇提取,提取液经减压蒸馏至干,再用甲醇溶解，然后吸附于硅胶上,并以不同体积比的氯仿-甲醇混合液按洗脱剂的极性由小到大进行洗脱,以RP-HPLC法检测洗脱液中物质的种类和含量。结果表明:洗脱剂为氯仿-甲醇（体积比为8∶1）的洗脱液经分析为单一组分,其保留时间为5.142 min；以对照品京尼平甙酸添加法测定,其峰高增加；相关紫外光谱和红外光谱检测结果与京尼平甙酸对照品基本一致；结合LC-ESI-MS、 1H-NMR和13C-NMR等测定，确定该洗脱组分为京尼平甙酸。