色谱

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新型微填充柱－毛细管柱色谱操作条件的优化及灰色关联分析

许国旺,国振双,杨黎,周申范,张玉奎,卢佩章

1995, 13 (4): 235-237.

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通过正文设计实验方法优化了新型微填充柱。毛细管柱色谱操作条件，并利用灰色关联分析方法考察了操作条件与柱效的相关程度，对实验能起一定的指导作用。

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用免疫亲和柱分离、高效液相色谱法测定花生和玉米中黄曲霉毒素的研究

王光建,何才云,鲁长豪,赵建忠,王勇

1995, 13 (4): 238-240.

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建立了用免疫亲和柱分离净化、高效液相色谱法测定花生和玉米中黄曲霉毒素（ＡＦＴ）Ｂ＿１、Ｂ＿２、Ｇ＿１、Ｇ＿２的方法。采用６０％甲醇提取样品中的ＡＦＴ，氢氧化铁沉淀吸附除去样品液中大部分杂质，再经过亲和柱将ＡＦＴ截留，进一步与杂质分离，洗脱后，加三氟乙酸衍生化处理，反相高效液相色谱法分离定量。对样品中四种ＡＦＴ的最低可测下限浓度均为１μｇ／ｋｇ，样品加标５～１０μｇ／ｋｇＡＦＴ，回收率在７６．９％～１１３．６％范围内。

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利用高效弱阴离子交换色谱法纯化超氧化物歧化酶

郑莹,周信基,李华儒

1995, 13 (4): 241-243.

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利用高软弱阴离子交换色谱法简化了超氧化物歧化酶（ＳＯＤ）的纯化手续。在丙酮沉淀后，仅用一步色谱分离就能使来自牛血的Ｃｕ，Ｚｎ－ＳＯＤ达到电泳纯，活性回收率为８６．４％，比活为７７１１Ｕ／ｍｇ，纯化倍数提高至５２倍。此外，详尽讨论了色谱分离的条件。

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单糖、多元醇亚砷酸络合物毛细管电泳分离研究

任吉存,邓延倬,程介克

1995, 13 (4): 244-246.

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采用激光干涉检测方法系统研究了单糖、多元醇亚砷酸络合物的电泳行为；并考察了溶液中ｐＨ值、亚砷酸盐浓度对单糖、多元醇亚砷酸络合物淌度的影响。实验结果表明，在亚砷酸溶液中，单糖和多元醇的选择性好，峰形尖锐；从而建立了一种单糖、多元醇毛细管电泳分离及直接检测的新方法。

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高效毛细管电泳测定黄连及成药中小檗碱型生物碱的含量

张国华,王延琮,张永友,王磊,张玉奎

1995, 13 (4): 247-249.

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报道了黄连及成药中七种小檗碱型生物碱的高效毛细管电泳分离测定方法。缓冲液由６５％磷酸氢二钠（用磷酸调ｐＨ７．０）和１５％甲醇组成。方法具有良好的精密度、回收率及线性关系。并用此法定量测定了黄连及六种成药中三种生物碱（小檗碱、巴马汀、药根碱）的含量。

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光学活性高分子的手性固定相

陈传福,任长玉,习复

1995, 13 (4): 250-253.

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光学活性高分子的手性固定相

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毛细管电泳的原理及应用第一讲毛细管电泳简介

罗国安,王义明

1995, 13 (4): 254-256.

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毛细管电泳的原理及应用第一讲毛细管电泳简介

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激光诱导荧光检测器──一种高灵敏度的高效液相色谱和毛细管电泳检测器

马明生,韩慧婉,刘国诠

1995, 13 (4): 257-261.

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Laser induced fluorescence(LIF)detector as a highiy sensitive detector for HPLC and HPCE was widelyused in biochenllcal analysis,DNA sequencing,immunoassay,etc.In the present paper a review of LIF forHPLC and HPCE was reported with 48 references. The principles for choice of the components contained in aLIF detector,such as,a lase,optic lens,filters and a photodetector,were reviewed in detail.Various opticdesigns and detection flow cells were also reviewed.

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双柱双泵高效液相色谱－电化学法测定尿中香草扁桃酸

赵飞浪,袁倚盛

1995, 13 (4): 262-263.

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采用双柱、双泵和双阀，通过住切换技术对尿中的香草扁桃酸（ＶＭＡ）进行直接进样分离，并用电化学检测器检测。样品先进入柱Ⅰ，初步分离后，包含ＶＭＡ的组分被切换入柱Ⅱ进一步分离。结果显示，此法操作简单、快速，回收率高，重复性好。

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两种棉酚旋光体在碳十八柱上的分离

杨伟华,项时康

1995, 13 (4): 264-266.

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利用Ｌ－苯基丙胺醇与样品中的左旋（一）棉酚和右旋（＋）棉酚充分反应以后，对生成的两种棉酚衍生物进行高效液相色谱分析。该方法以ＷａｔｅｒｓμＢｏｎｄａｐａｋＣ＿（１８）色谱柱为固定相，甲醇－磷酸水溶液为流动用，获得了良好的分离效果。

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锆和铪的色谱分离

梁泽斌,王成智

1995, 13 (4): 267-268.

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介绍了用二甲基硅酮作固定相的毛细管气相色谱法分离三氟乙酰丙酮合锆和三氟乙酰丙酮合铪的混合物及乙酰丙酮合锆和乙酰丙酮合铪的混合物。用Ｃ＿（１８）键合固定相的反相高效液相色谱法分离上述β－二酮合锆和铪的混合物；讨论了色谱分离中的问题。

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气相色谱法用于分枝杆菌脂肪酸组成与菌种鉴定的研究

康建,马小锋,包美复,侯晓娜

1995, 13 (4): 269-271.

摘要 ( 1529 ) [Full Text(HTML)] ()

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采用非极性毛细管柱气相色谱法对３株分枝杆菌细胞脂肪酸化学组成进行了研究，得到特异性指纹识别图，并对７例临床分离的分枝杆菌进行了鉴别。结果表明，结核菌硬脂酸（ＴＳＡ）为分枝杆菌属的特征组分，其含量与其他中长链脂肪酸的百分组成随菌种不同而异。

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用色谱联用技术分析桂腈和溴代苏合香烯顺反异构体

许宏琪,盛龙生,安登魁

1995, 13 (4): 272-273.

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应用气相色谱／红外光谱（ＧＣ／ＦＴＩＲ）、核磁共振（ＮＭＲ）等技术快速分离、鉴定了桂腈和溴代苏合香烯的顺反异构体，解决了气相色谱／质谱（ＧＣ／ＭＳ）分析时出现的保留行为不同的顺反异构体因为质谱图类似而导致谱库检索鉴别困难的问题。从而，可将保留指数与质谱数据相结合，互补各自在鉴定上的局限性。

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裂解毛细管柱气相色谱－傅里叶变换红外光谱的剖析应用

钟山,冯子刚

1995, 13 (4): 274-276.

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采用裂解气相色谱－傅里叶变换红外光谱（ＰｙＧＣ／ＦＴＩＲ）技术，使用大口径毛细管柱，分析了一未知进口涂料，对其主要裂解碎片峰进行了定性，进而从特征碎片的产生推出该涂料的成分。并同常规红外光谱差减法进行了比较，结果表明ＰｙＧＣ／ＦＴＩＲ具有简便、快速、全面和无需标样等优点，有广泛的应用价值。

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牛蒡子中木脂素的薄层扫描测定

李慧义,罗淑荣

1995, 13 (4): 277-278.

摘要 ( 1438 ) [Full Text(HTML)] ()

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在高效硅胶薄层板上分离了牛蒡子中４种２，３－苄基丁内酯型木脂素──牛蒡甙元（Ｉ）、牛蒡素Ｂ（Ⅱ）、牛蒡酚Ａ（Ⅲ）、牛蒡酚Ｆ（Ⅳ）。流动相为二氯甲烷－乙醚－甲醇－己烷（４：１：０．４：１），室温放置，自然显色。薄层扫描法定量，各木脂素的线性范围在０．４５１～４．６０８μｇ，回收率为９９．９０％～１００．９０％，并用此法测定了不同产地牛蒡子中木脂素的含量。方法简便、快速，样品用量少。

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甾体药物薄层色谱分析数据库

蔡红,孙毓庆

1995, 13 (4): 279-280.

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利用ＴＵＲＢＯＰＲＯＬＯＧ程序设计语言，建立了一个甾体药物薄层色谱分析数据库，收集了中国药典一九九０年版、英国药典一九八八年版及美国药典第二十二版中甾体原料药及其制剂的薄层色谱数据，为甾体药物的薄层色谱分析提供了方便。

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大口径毛细管柱气相色谱法分析三氯杀螨醇

毕富春,王文丽

1995, 13 (4): 281-283.

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A method of quantitative analysis for dicofol by a wide bore capillary column has been studied. The gaschromatographic conditions were as follows.Column:fused silica, HP-1(cross-linked methyl silicone)5m ×0.53mm × 2.65μm film;column temperature : 200℃;temperature of injector and detector: 250℃ and carriergas:H_2 25mL/min. Dioctyl phthalate was used as the internal standard.10% of dicofol would be decomposedquantitatively to dichlorobenzophenone.

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气相色谱法（毛细管柱和填充柱）测定农作物中增塑剂DEHP的残留量

杜荣平,庞金梅

1995, 13 (4): 284-285.

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This paper describes the determination of the plasticizer DEHP residues in plants and seeds of crops bygas chromatography with capillary and packed columns. DEHP recovery rate was over 90%with high-speedand low cost.This method,especially with packed column is very suitable for the determination of phthalates.

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心脏手术中心肌组织高能磷酸化合物的高效液相色谱测定及比较研究

刘智敏,东云华,寇瑛莉

1995, 13 (4): 286-287.

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High-energy phosphate compounds from myocardial tissues were deternuned by HPLC with LichrosorbRP18 as stationary phase and phosphate buffer as mobile phase. The myocardial tissues were taken from car-diac patients whose hearts were perfused with cold crystalloid cardioplegia(CCC),cool blood cardioplegia(CBC)and warm blood cardioplegia(WBC) in cardiac surgery. The analytical results showed that CBC andWBC are superior to CCC in energy charge of myocardial tissue and will be used in cardiac surgery.

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高效液相色谱法同时测定肿瘤患者尿中假尿苷和肌酐的含量

何书泉,韩跃武,朱昕,李亢宗,魏睛霞

1995, 13 (4): 288-289.

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An HPLC method for the simultaneous determination of pseudouridine(Pu)and Cretinine(C)in urinewas established;The recoveries of Pu and C were 92. 09±3.5%and 83. 01±5.7%respectively. The calibra-tion curves were linear within the concentration range of 2～200μg/mL for Pu and 5～300μg/mL for C. The detection linilts for Pu and C were 2. 15μg/mL and 4.75μg/mL. The method is rapid,sensitive and reliable.

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高效液相色谱法测定22S，23S，24R表高油菜素内酯

刘国清,张洪彬,刘建平,李良

1995, 13 (4): 290-291.

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The sample was dissolved in ethyl acetate and reactcd with pbenylboronic acid at 80°for 3Omin.Then itwas detemined by HPLC using UV detector at 222nm. The linear relations between the amounts and thepeak areas in the range of 0. 02mg/mL to 0.12mg/mL were staisfactory(γ=0. 9999,n=6). Average recovery was 99.27%～101.5%.

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高效液相色谱法测定联苯取代衍生物的三种异构体

尤进茂,孙学军,郑庚修,卢常源

1995, 13 (4): 292-294.

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A method for the separation and deternunation of three isomers of 4-nitro-methyldiphenyl by reversed-phase HPLC is described.The method for quantitative analysis without standard substance was studied with satisfactory results.

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薄层色谱法分离测定辣椒红色素中的辣椒红

丁来欣，陈里

1995, 13 (4): 295-296.

摘要 ( 1229 ) [Full Text(HTML)] ()

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丙烯醛－乙烯基乙醚法合成戊二醛工艺中的气相色谱分析

崔庆新,尹宝霖,张立云

1995, 13 (4): 297-299.

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2-Ethoxy-3,4-dihydropyran(I) is the intermediate in the synthesis of glutaraldehyde(II)Diels-Alderreaction of acrolein and vinyl ethyl ether. Both (I) and (II) can be analyzed successfully by gas chromato-graphy with a 2m column of 10% PEGS /Chromosorb W AW DMCS.

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松节油催化水化混合物的气相色谱分析

朱洁民

1995, 13 (4): 300-300.

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In industry,terpineol is obtained from catalytic hydration of turpentine oil. The products in this reactionare very complicated so that it is difficult to monitor the reaction process. By using GC with PEG-20M col-umn under temperature programnung condition,the author analysed the hydrated mixtures of turpentine oil. The separation of isomers of turpentine oil or terpineol and the precision of quantitative analysis are good.

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N－甲基吡咯烷酮、α－吡咯烷酮合成物系气相色谱分析

邱立勤,米镇涛,张香文

1995, 13 (4): 301-302.

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This paper describes a GC analytical method in the synthes is of N-methyl pyrrolidone of a-pyrrolidone.This procedure was performed with a column packed with 6%OV-17/silanized 101 support and FID detec-tor. Calibration factors and detection conditions are given,The coefficients of variation of NMP and a-P were0.6%and 0.5%respectively. The relative errors of all the components were not more than±3.0%,Thequantitative analysis is fast,simple and accurate.

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扑杀特的高效液相色谱分析

向文胜,苏少泉,马英,王晴

1995, 13 (4): 303-304.

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An RP-HPLC method for the quantitative deternunation of imazethapyr in technical product and formula-ion has been developed. Operating conditions were YWG-C18 colunmn,25cm×5.0mm i.d,methanol-water-glacial acetic acid(80 : 20: 1. 2 ,volume ratio) eluent and UV-254nm dstection.The method is reproducibieand the coefficient of variation was less than 1.5%.

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反相高效液相色谱法测定药物“金水宝”中腺苷及腺嘌呤含量

李来生

1995, 13 (4): 305-306.

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A method for determining adenosine(A)and adenine(B)in the drug of Jin Shui Bao by RP-HPLC on μ- Bondapak C18 (3.9mmi.d. ×300mm) using 0. 01mol/L KH_2PO_4- methanol(85 :15,V/V,pH 5.7 )as themobile phase(1. 5mL/min )is described in this paper. The UV detector was set at 254nm. Aand B were ex-tracted with 0. 01%acetic acid Recover1es were 97. 18%～101.92%for A and 98.35%～101.19% for B. The method is simple,rapid and accurate.

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