色谱

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高连存,崔兆杰,张春阳,王淑仁

1996, 14 (1): 1-4.

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详细系统地研究了收集溶剂的种类、用量及无溶剂固体表面冷冻捕集等方法对离线收集超临界流体萃取多环芳烃组分效率的影响。研究发现，二氯甲烷和丙酮的收集效率较高，其回收率为６１．４４％～１０５．４０％，其它有机溶剂效果较差。而且，当收集溶剂的液面高度大于２．０ｃｍ时，溶剂的用量对收集效率没有明显的影响。玻璃珠固体表面冷冻捕集效果较好，其回收率在６０．９８％～１０９．８８％之间，但其精密度较差，相对标准偏差（ＲＳＤ）在０．２８％～１１．２９％之间。

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用气相色谱法研究乙酸乙烯酯不对称氢甲酰化反应中溶剂的影响

黄撷云,杨世琰,何春燕

1996, 14 (1): 5-9.

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用毛细管气相色谱、色－质谱和旋光色散及圆二色性谱仪等方法对乙酸乙烯酯在非极性和极性溶剂中的不对称氢甲酰化反应产物进行分离和鉴定。实验结果表明，在非极性溶剂中反应的收率、选择性、光学收率ｅ．ｅ．值（ｅｎａｎｔｉｏｍｅｒｉｃｅｘｃｅｓｓ）均比极性溶剂中的结果为好。由此探讨了不对称氢甲酰化反应中溶剂的影响。

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重质石油中含氮化合物的形态及分布分析──高效液相色谱－气相色谱在线联用分析方法研究

胡坪,孙科夫,陈卫东,朱明华,郑永杰

1996, 14 (1): 10-13.

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研究了高效液相色谱－气相色谱（ＨＰＬＣ－ＧＣ）联用技术及其应用。采用正相微柱ＨＰＬＣ－ＧＣ联用及完全溶剂蒸发方式，分析了煤焦油馏分──蒽油，显示了微柱ＨＰＬＣ－ＧＣ联用的应用潜力。采用正相ＨＰＬＣ－ＧＣ联用结合反冲技术，分离了重质石油中的饱和烃、芳烃和极性化合物（含氮化合物等）。

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高效液相色谱法测定动物脑和脊髓内微透析样品中的递质氨基酸和单胺类递质及其代谢产物

叶惟泠,尹萍波

1996, 14 (1): 14-17.

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测定了猴、兔的尾核、海马和小脑深核以及猫脊髓背角微透析样品中递质氨基酸和单胺类递质及其代谢产物的含量。浓度与响应的线性关系、检测极限和重复性均与以前的报道一致。对应用常规液相色谱方法分析脑内微透析样品中的上述化合物时应注意的问题作了扼要的讨论。

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高效液相色谱法制备人胆汁中结合胆红素

涂向群,祝学光,韩健德

1996, 14 (1): 18-21.

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针对单结合胆红素（ｍｏｎｏｃｏｎｊｕｇａｔｅｄｂｉｌｉｒｕｂｉｎ，ＭＣＢ）理化性质极不稳定而造成对其分析、制备的困难性，在Ｓｐｉｖａｋ和Ｔｒｏｔｍａｎ方法的基础上建立了一个简单可行的人胆汁结合胆红素（ｃｏｎｊｕｇａｔｅｄｂｉｌｉｒｕｂｉｎ，ＣＢ）高效液相色谱（ＨＰＬＣ）二次洗脱的制备方法，并对方法的可靠性作了论证，得到了ＭＣＢ较为满意的量与纯度，为进一步探讨ＭＣＢ的理化性质及其与胆石形成的关系提供了条件。

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新型微填充柱－毛细管柱二维色谱系统过程的动力学研究

张维冰,许国旺,史景江,杨黎,张玉奎,卢佩章

1996, 14 (1): 22-26.

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从色谱动力学角度对新型微填充柱－毛细管柱二维色谱系统过程中双柱条件与流出曲线及柱效之间的依赖关系加以系统研究。结果表明：由于双柱条件之间存在关联，双柱系统流出曲线特征与单柱系统存在一定的差异，流出曲线一阶矩和二、三阶中心矩以及双柱系统的柱效皆由预柱和主柱条件综合确定。

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交联XE－60和PEG－20M极性固定相非晶硅膜改性弹性玻璃毛细管柱研究

张桂琴,齐兴义,杨正华,郑国栋,刘恒秋

1996, 14 (1): 27-29.

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研究了交联ＸＥ－６０和ＰＥＧ－２０Ｍ极性固定相非晶硅膜改性弹性玻璃毛细管柱，在适当的温度下，用过氧化二异丙苯（ＤＣＵＰ）游离基引发交联，成功地制备了ＸＥ－６０和ＰＥＧ－２０Ｍ极性柱，它们均具有柱效高、惰性好、化学稳定性好和耐溶剂、抗腐蚀、耐高温等性能，是一种新型的极性交联柱。

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扇贝脂肪的提取和分析

张强

1996, 14 (1): 30-32.

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以快速脂肪提取法取代素氏提取法，提取扇贝脂肪仅需４５ｍｉｎ，提取率９８．８％。利用４０ｍ×０．３５ｍｍｉ．ｄ．ＰＥＧ－２０Ｍ玻璃毛细管柱分离测定扇贝脂肪中脂肪酸。分离出４６个峰，结合气相色谱／质谱（ＧＣ／ＭＳ），鉴定出３６个峰，占脂肪区总量的９９．４％，其中饱和脂肪酸占３２％，不饱和脂肪酸占６７．４％。

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气相色谱－原子发射光谱联用仪测定18种安眠镇静药的元素比例及其在中毒病人全血样品中的应用

顾明松,冯翠玲,罗毅

1996, 14 (1): 33-36.

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采用气相色谱－原子发射光谱联用仪（ＧＣ－ＡＥＤ）测定了１８种安眠镇静药的元素组成和元素比例。根据气相色浴－质谱（ＧＣ－ＭＳ）测定的分子量数据推测出它们的分子式，结果与实际值一致。以元素组成、元素比例和保留时间为判据，对一例中毒患者全血样品进行了定性分析，发现血中含有苯巴比妥。

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环境水质中酚类优先监测物的气相色谱法测定

李新纪

1996, 14 (1): 37-40.

摘要 ( 1637 ) [Full Text(HTML)] ()

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以气相色谱法（ＧＣ）测定了环境水质中的重点酚类污染物。选择乙酸酐作衍生化试剂、甲苯为萃取剂，比较了不同的衍生ｐＨ条件，给出了氢火焰离子化检测器（ＦＩＤ）分离测定酚类污染物的精密度和检出限。方法简便实用，经５家实验室验证表明：适用于监测地表水和污水中的酚类物质。６种酚类优先监测物的检测限为０．６～７μｇ／Ｌ。

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含磷毒剂及其降解产物的气相色谱-质谱测定方法研究

顾惠芬，周黎明，蔡冠梁，钟玉征

1996, 14 (1): 41-44.

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研究了用台式气相色谱-质谱仪分析测定含磷毒剂及其降解产物，并对降解产物的衍生化方法及它们的色谱行为进行了研究，总结分析了它们的质谱裂解特点及规律，测定了水样中的含磷毒剂及降解产物。

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气相色谱中测定死时间的Grobler－Balizs法和Ambrus法的比较

吴宁生,苏红伟,史文娟

1996, 14 (1): 45-46.

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经理论推导和实验数据验证，证明测定死时间的Ｇｒｏｂｌｅｒ－Ｂａｌｉｚｓ法和Ａｍｂｒｕｓ法是同一的。

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PICO-TAG反相色谱法测定鸡蛋中氨基酸含量

尚素芬，王洪

1996, 14 (1): 47-49.

摘要 ( 1383 ) [Full Text(HTML)] ()

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采用PICO-TAG反相色谱法测定了氨基酸，方法的相对标准偏差为0.75％，平均回收率为97.12％。对鸡蛋样品进行了测定，发现不同产地不同皮色鸡蛋中氨基酸含量无显著差异，样品测定相对标准偏差为1.67％。结果表明测定方法快速、灵敏、准确、重现性好。

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离子排斥色谱法测定马齿苋中低分子羧酸

郜志峰,刘鹏岩,傅承光

1996, 14 (1): 50-52.

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以２．０ｍｍｏｌ／Ｌ对甲苯磺酸为淋洗液，用非抑制型电导检测离子排斥色谱法测定了马齿苋叶及茎中的柠檬酸、丙二酸、苹果酸、抗坏血酸、琥珀酸、反丁烯二酸和乙酸。

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气相色谱法测定线虫中的脂肪酸含量

郑文晖,谭炳炎,汤丽芬,李章旺

1996, 14 (1): 53-55.

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ematode is a small organism and the traditional purification method needs a lot of nematodes , but it is difficult for us to foster many nematodes.The fatty acids in nematode were esterified directly in our analytical method,so that,the error is reduced the and sensitivity is improved. The results showed that thisimproved analysis method could be used for rapid and satisfactory determination of the fatty acid change during storagr of this group of nematodes.

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气相色谱法分析不同提取条件的海狸鼠油脂成分

叶非,王静,宫百揆,葛蔚,冯志彪

1996, 14 (1): 56-57.

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The fat and oil from myocastor coypus have been analysed by gas chromatography. Eight components were identified with a rapid and reliable method. Chromatographic conditions were as follows:column,10% DEGS on Chromosorb W AW DMCS(60 - 80 mesh),1.3m × 3.0mm i.d.;column temp.,195℃;injection temp.,250℃;detector temp,.250℃;carrier gas N2 with flow rate of 35mL/min.

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高效液相色谱法在青霉素生产工艺中的应用

关一鸣,王常青,刘志强,李秀伟,王刚毅,付亚萍

1996, 14 (1): 58-59.

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A method of simutaneous determination of phenylacetic acid and peniciline in manufacture by high performance liquid chromatography has been proposed.The effective value of peniciline and content of phenylacetic acid in ferment solutions of different periods in production were measured.The method is accurate,convenient and fast.

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高效液相色谱法测定家兔血清中盐酸山莨菪碱含量

周宏兵,张?,何新

1996, 14 (1): 60-61.

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rapid method for the separation and determination of anisodamine hydrochloride in serum of rabbit has been developed with Nucleosil column of 4. 6× 250mm and CH3OH-H2O-(C2H5)3N (30:70 : 0.125)as mobile phase. Anisodamine hydrochloride was determined by reversed phase HPLC at 214nm.Atropine sulfate was used as an internal standard. The calibration curve was Y= 0.01945X+0. 05623,r= 0. 9998,n= 6.It was rectilinear within the range between 0. 75μg/mL-50.0μg/mL,and the recovery was from 97. 0% to 98. 2%.

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木素碱性硝基苯氧化产物的高效液相色谱分析

马文秀,吴伟志

1996, 14 (1): 62-63.

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- hydroxybenzaldehyde,vanillin and syringaldehyde etc. were separated on a Novapak C18 column (5μ 3. 9mm i. d.× 150mm) and eluted with MeOH-H2O (25:75, V/V) at a flow rate of 0. 6mL/min and detected at 254nm. Quantitative analysis was performed with piperonal instead of synthetic product . m-meconin,as the internal standard. Recoveries are 95%-98% and CV≤1%. The method is simple,rapid and reliable.

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血清中阿斯匹林和水杨酸浓度的快速高效液相色谱法测定

孙长海,王敏

1996, 14 (1): 64-65.

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A fast method for determining concentrations of aspirin and salicylic acid in serum using reversedphase high performance liquid chromatography with Spherisorb C18 column,MeOH i H2O: n-BuOH : H3PO4 (300:200 :10 :0. 5,volume ratio) eluent and UV-237 detector was eatablished. The linear range of the method is 1-20μg/mL (r=0. 9996)for aspirin and 2 30μg/mL (r=0. 9981) for salicylic acid. The averagerecoveries are 96. 0 %-106. 0% and 92. 0%-119.5% ,respectively.

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气相色谱法测定三环氧丙基异氰尿酸酯中环氧氯丙烷残留量

茅力,练鸿振,戴建国,苗进

1996, 14 (1): 66-66.

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A simple,rapid and reliable method for the determination of trace epichlorohydrin residue in tris (2 ,3-epoxy propyl) isocyanurate for industrial use by gas chromatography is described. The gas chromatographic separation was achieved on a glass colunin packed with 4% SE-30/Chromosorb W HP at a column temperature of 80℃.The detector was FID and the carrier gas was N2.Three preducts from various manufacturers were analyzed by this methed with the coefficient of variation of 2. 2%-5. 2%。

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气相色谱法测定除草剂吡嘧黄隆

郭兴杰

1996, 14 (1): 67-68.

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A gas chromatography method for the quantitative analysis of pyrazosulfuron is described. Analytical conditions were as follows:column:OV-225 (5% )on Chromosorb W AW DMCS(60-80 mesh),2m column with 3mm i.d.at 172℃;FID at 260℃;N2 as carrier gas with flow rate of 30mL/min.

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气相色谱法定量分析α－乙酰－γ－丁内酯

潘奉华,朱京科,骆有寿,孙昊

1996, 14 (1): 69-70.

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?Butyrolactone, α-acetyl-γ-butyrolactone and solvent in reaction mixtures from the preparation of α-acetyl-γ-butyrolactone were determined by gas chromatography.The analytes were separated at 190℃ on a 1m ×3mm stainless-steel column packed with silanized 102 white support coated with polydiethylene glycol succinate and monitored with a thermal conductivity detector. The relative error was less than 2.5%.

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液相色谱法分离大麦籽粒中的原花色素

王建清,杨煜峰,褚建新

1996, 14 (1): 71-72.

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A method for the separation of proanthocyanidins in barleycoms by high performance liquid chromatography with ODS column and aqueous-methanol as eluent has been reported.

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反相高效液相色谱法测定豆黄隆可湿性粉剂

何悠崎,黄信江

1996, 14 (1): 73-74.

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n RP-HPLC method for quantitative determination of chlorimuron ethyl WP in technical product and formulation was developed.Operating conditions were YWG-C18 column, 220×4. 6mm, methanol-waterethyl acetate (2:2 :1 ,volume ratio) mobile phase and UV detection at 254nm.The results showed that the recoveries were between 99.44%-99.93% and the coefficient of variation is less than 0. 16%. The method is simple,rapid and very effective.

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马铃薯体内腺嘌呤代谢物的薄层色谱法

乌云，李秉真，田瑞华，索兰弟，刘梦云

1996, 14 (1): 75-76.

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正相高效液相色谱法测定辛硫磷、顺式氰戊菊酯和灭多威

王以燕,孙百忠

1996, 14 (1): 77-78.

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eterminations of phoxim,esfenvalerate and methomyl were carried out by using normal-phase HPLC in two different mobile phase conditions with UV detector(at 254nm).The results showed that the separation of the above-mentioned compounds was satisfactory.The CV of phoxim,esfenvalerate and methomyl were 0.43%,3.05% and 0. 55% respectively.This method is simple ,rapid ,sensitive,accurate and meets the demand of quantitative analysis.

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气相色谱法测定甲苯氧化产物中的苯甲醛及苯甲酸

刘敬兰,周鸿娟,陈连文,傅德才

1996, 14 (1): 79-80.

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气相色谱法测定甲苯氧化产物中的苯甲醛及苯甲酸刘敬兰，周鸿娟（河北师范大学实验中心石家庄０５００１６）陈连文傅德才（河北经贸学院石家庄０５００６１）（河北轻化工学院石家庄０５００１８）１前言在由电化学间接氧化法从甲苯生产苯甲醛的反应过程中，反应条件及终点的控制直接影响着苯甲醛的回收率。苯甲醛及苯甲酸的测定方法虽已有报道〔１〕，但同时测定甲苯中两组分含量的方法尚未见报道。２实验部分（１）色谱条件：岛津气相色谱仪ＧＣ－１６Ａ，带Ｃ－Ｒ３Ａ数据处理机。

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