高效液相色谱法测定全血环孢霉素A的浓度

建立了高效液相色谱法测定全血环孢霉素Ａ 浓度的方法。全血样品经多步处理后以２０ μＬ注入ｒｅｏｓｏｌｖｅ Ｃ１８,５μ色谱柱,采用Ｖ（乙腈）∶Ｖ（水）＝ ８０∶２０ 的流动相,在７５℃柱温下,以１ ｍ Ｌ／ｍ ｉｎ 流速洗脱,检测波长为２０８ｎｍ 。环孢霉素Ａ 的回收率为９９％ ～１０４ ％ ,相对标准偏差＜ ３．４２％ （ｎ＝ ５） ,日间＜ ８．１９％ （ｎ＝ ４） 。最低检测浓度为２５ μｇ／Ｌ。     

高效液相色谱法测定大鼠血浆和全血中核黄素的含量

为了直接反映核黄素营养状况对血中核黄素水平的影响,建立了高效液相色谱测定大鼠血浆及全血中核黄素含量的方法。采用Diamonsil C 18 色谱柱(250 mm×4.6 mm i.d.,5 μm)分离,以甲醇-5 mmol/L 乙酸铵(体积比为35∶65)为流动相,流速1.2 mL/min ,荧光检测器检测(激发波长:450 nm,发射波长:520 nm)。样品经乙腈、三氯甲烷处理后进样分析。核黄素测定的线性范围为5～200 nmol/L ,最低检测限为2.5 nmol/L (S/N＝2),日     

高效液相色谱-荧光检测法同时测定全血中5种香豆素类杀鼠剂

建立了同时测定全血中杀鼠灵、杀鼠迷、溴敌隆、氟鼠灵与溴鼠灵等5种香豆素类杀鼠剂的简便、灵敏、准确的高效液相色谱-变波长荧光分析方法。全血样品经乙酸乙酯提取后,在XDB C18柱(150 mm×2.1 mm, 5 μm)上以甲醇-0.2%乙酸水溶液(体积比为88∶12)混合液为流动相,采用荧光变波长程序检测,同时通过建立各杀鼠剂的荧光光谱库,利用谱库检索,提高定性的准确度。各杀鼠剂的线性范围为0.01~10.00 mg/L（杀鼠灵为0.05~10.00 mg/L）,检出限为0.01~0.05 mg/L,方法的加标回收率为81%～98%,其相对标准偏差（RSD）为3.8%～8.5%。该法适用于中毒病人的中毒诊断检测。     

用GC－MS法测定尿中可待因及其代谢物的浓度

建立了用ＧＣ－ＭＳ（ＳＩＭ）内标定量法快速测定人尿中可待因及其代谢物浓度的方法。样品经酸水解、乙醚／异丙醇提取，用ＭＳＴＦＡ－ＭＢＴＦＡ衍生化后进样于ＧＣ－ＭＳＤ，方法灵敏、准确，可用于监测吸毒者尿中可待因、吗啡类药物的浓度。本法已经受ＩＯＣ的１９９２年水平考试的考验。     

高效液相色谱法测定大鼠血浆中的原儿茶酸

建立了大鼠血浆中原儿茶酸含量测定的高效液相色谱方法。采用的色谱柱为DiamondsilTM C18 柱(150 mm×4.6 mm,5 μm);流动相为乙腈-水(体积比为9∶91,用H3PO4 调pH至2.5);流速1.2 mL/min;检测波长260 nm;内标为对羟基苯甲酸。原儿茶酸的线性范围为0.050~3.20 mg/L,线性相关系数为0.9978，最低定量限为0.050 mg/L,日内和日间测定的精密度（以相对标准偏差表示）均低于7.0%,准确度（以相对误差表示）为-1.4%～2.6%；在0.050,0.40,3.20 mg/L低、中、高3个添加浓度水平下，血浆样品的提取回收率分别为83.4%,87.3%,91.1%。该方法简便,灵敏,准确,适用于大鼠体内原儿茶酸的药物动力学研究。     

高效液相色谱法测定血中苯妥英浓度

A high performance liquid chromatographic method for the quantitative analysis of phenytoin(PHT) inhuman plasma or whole blood is described. After a onestep extraction of PHT and internal standard withethyl acetate from human plasma or whole blood,samples were chromatographed on a Spherisorb-C(18) columnwith a mobile phase of methanol-water-tetrahydrofuran(45/55/5,V/V/V)at a flow rate of 0. 3mL/min. Theeluant was monitored at 210nm.     

高效液相色谱法测定全血中骨碱性磷酸酶的活力

 建立了测定全血中骨碱性磷酸酶(BALP)的高效液相色谱法(HPLC)。色谱柱为SpectraPhysicsODS反相柱,以V(0.01mol/L乙酸,pH4.8)∶V(甲醇)=70∶30的溶液为流动相,流速为0.8mL/min,检测波长为275nm。当BALP的质量浓度为8～200mg/L时,其活性对峰面积呈良好的线性关系(r=0.996),检测限为3ng。该方法简便、快速、可靠,可用于临床测定全血中的BALP。     

Rapid Analysis for Codeine by Reversed-Phase High-Performance Liquid Chromatography

Abstract

A reversed phase high-performance liquid chromatographic (HPLC) method has been established for the separation and quantitative determination of the alkaloid codeine in pharmaceutical preparations and in body fluids. The minimum detectable concentrations for body fluids were 5ppb and 7ppb respectively for urine and whole blood with an analysis time of under 5 min. A RP-8 Spheri-5 guard column and a RP-8 Lichrosorb-10 column were used and codeine was detected at its absorption maximum wavelength of 212 nm using an eluting system of methanol: 0.5% w/v aqueous ammonium acetate (70:30) at a pH of about 7.0.     

Surfactant-to-Dye Binding Degree Method for the Determination of Morphine Hydrochloride and Codeine Phosphate in Pharmaceuticals

Abstract

The surfactant-to-dye binding degree method was used to determine morphine hydrochloride and codeine phosphate. Neutral red and bis(2-ethylhexyl) sulfosuccinate (AOT) were used as the dye and surfactant, respectively, to form dye–surfactant aggregates. Addition of the drug resulted in a decrease in the dye–surfactant binding degree, proportional to the drug concentration. This was measured by monitoring the absorbance changes of the dye at 532 nm. Under the optimum conditions, the calibration graphs were linear up to 32 and 28 µg mL^?1 for morphine hydrochloride and codeine phosphate, respectively, with the corresponding detection limits of 0.40 and 0.35 µg mL^?1.     

吗啡和海洛因等生物碱的高效液相色谱化学发光测定

研究了吗啡、可待因、Ｏ＾３单乙酰吗啡和海洛因等生物碱在多聚磷酸介质中与高锰酸钾的发光行为和光谱现象。建立了反相 高效液相色谱化学发光检测吸毒者尿液和雅片中吗啡、可待因等物质的方法。     

Determination of Unbound Ampicillin in Rat Blood by Microdialysis and Liquid Chromatography

ABSTRACT

An in vivo microdialysis sampling method coupled to high-performance liquid chromatography has been applied for continuous monitoring of unbound ampicillin in rat blood. A microdialysis probe was inserted into the jugular vein/right atrium of Sprague-Dawley rats, and doses of 100 and 200 mg/kg ampicillin were then administered via the femoral vein. Dialysates were collected and directly injected into a liquid chromatographic system. Isocratic elution of ampicillin was achieved within 10 min using the liquid chromatographic system. The chromatographic mobile phase consisted of methanol-100 mM monosodium phosphoric acid (25:75, v/v, pH 5.5). The wavelength of the UV detector was set at 230 nm. The calibration curves from 0.25 to 50 μg/ml were linear with correlation coefficients of 0.995. The method provides a simple technique for rapid analysis of unbound ampicillin in rat blood for used in pharmacokinetic study.     

高效液相色谱法对吗啡、杜冷丁、安定的同步测定

利用高效液相色谱法同时分析测定了血液中吗啡、杜冷丁、安定的质量浓度。分析柱为C18,流动相为V（甲醇）：V（25mmol／LKH2PO4）＝90：10,检测波长为285nm。样品血液pH8．5～9．4时,用V（氯仿）：V（异丙醇）＝9：1溶液提取,以氮气吹干有机溶剂后用流动相溶解残渣进样分析。线性范围为0．05～50mg／L,最小检出质量浓度为0．05mg／L,日内与日间精密度CV＜6％。     

高效液相色谱—电化学检测法测定大鼠脊髓灌流液单胺类递质及其代谢产物

用反相离子对高效液相色谱－电化学检测法分离并同时测定了大鼠脊髓灌流液中部分单胺类神经递质及其代谢产物。选择了较为理想的色谱条件，使生物样品的检测限达到８０～６７０ｐｇ，单胺类递质代谢产物的回收率保持在８３％～１０６％范围内。     

全血中维生素E和辅酶Q10含量的高效液相色谱法测定

建立了一种同时测定全血中维生素E和辅酶Q10的高效液相色谱法.样品经乙醇沉淀蛋白,以正己烷萃取,氮气吹干后,流动相溶解,以甲醇-乙醇(体积比20 : 80)为流动相,在C18柱 (5 μm, 250 mm×4.6 mm i.d.)上进行色谱测定.维生素E和辅酶Q10的线性范围皆为1.0 ～50.0 mg/L,检出限分别为0.21、0.15 mg/L,相对标准偏差分别为5.2%、5.9%;全血样品的维生素E和辅酶Q10加标回收率分别为97%～115%和90%～112%.     

Determination of the Antimalarial Primaquine in Whole Blood and Urine by Normal-Phase High-Performance Liquid Chromatography

Abstract

A method has been developed to estimate primaquine in whole blood and urine by sensitive and selective high-performance liquid chromatography. Using the linear chain analogue of primaquine as the internal standard, a single-step extraction, normal-phase silica column with a basic mobile phase, levels down to 1 ng/ml of primaquine could be measured with good precision. Other anti-malarials like amodiaquine and pyrimethamine did not interfere in the assay. The major carboxylic acid metabolite of primaquine did not elute under the normal-phase chromatographic conditions. The method is suitable for use in clinical pharmacokinetic studies with primaquine.     

高效液相色谱法测定大鼠肝过氧化物酶体膜磷脂

 用 HPL C测定了过氧化物酶体膜磷脂的含量。用 Folch法提取膜脂质 ,以 μ-Porasil Si60为固定相 ,以乙腈-甲醇 -磷酸为流动相 ,采用梯度洗脱 ,紫外检测波长 2 0 5 nm。标准回收率 :心磷脂 (C)为 (1 0 3 .97± 1 2 .5 7) % ,磷脂酰肌醇 (PI)为 (88.2 3± 5 .42 ) % ,磷脂酰丝氨酸 (PS)为 (90 .3 3± 6.84) % ,磷脂酰乙醇胺 (PE)为 (84.41±1 0 .2 2 ) % ,磷脂酰胆碱 (PC)为 (89.78± 8.70 ) % ,鞘磷脂 (SM)为 (84.0 4± 1 2 .0 6) %。最小检出限分别为 :C1 2ng,PI 8ng,PS 2 3 ng,PE 4ng,PC 2 3 ng,SM 7ng。线性关系与回收率较好 ,结果令人满意。     

高效液相色谱/电化学法测定大鼠血液和脑组织中单胺类物质的含量

建立了高效液相色谱／电化学检测法测定大鼠脑组织和血液中单胺递质及其代谢产物的方法。能同时测定去甲肾上腺素（NE）、肾上腺素（E）、3,4-二羟基苯乙酸（DOPAC）、多巴胺（DA）、高香草酸（HAV）、5-羟色胺（5-HT）,并能和内标3,4-二羟卞胺（DHBA）分离良好。本方法快速、简便,回收率为92％-105％,线性范围2．8-680ng／mL,检出限为0．05ng（S／N=3）。本方法已应用在服用中药的大鼠下丘脑组织及血液的测定中,数据显示,本法能满足测定要求。     

反相高效液相色谱法测定鼠胆汁中游离与结合型胆汁酸

建立了一种柱前衍生反相高效液相色谱荧光检测大鼠胆汁中游离与结合型胆汁酸的方法.以4-溴甲基-7-甲氧基香豆素为衍生剂,月桂酸为內标,Waters Nova C18色谱柱分离,采用甲醇/乙腈和水梯度洗脱,荧光激发波长(λex)330 nm,发射波长(λem)400 nm,內标标准曲线法定量.各胆汁酸在5-2 400μmol/L范围内线性良好,r为0.998 9-0.999 7.最低检出限为1.2-2.5μmol/L.精密度日内在1.05%-3.67%之间,日间在3.16%-6.83%之间.平均回收率为87.8%-106.7%.该方法灵敏、重复性好,分析时间短,线性范围宽,适合于科研工作中对鼠胆汁中各胆汁酸进行定量检测.     

HPLC-APCIMS联用法测定全血中杀鼠迷

杀鼠迷(coumatetralyl)又称立克命,化学名为4-羟基-3-(1,2,3,4-四氢-1-萘基)香豆素,是一种慢性、广谱、高效、适口性好的第一代抗凝血类鼠药,其结构式如右所示。由于使用不当,造成人和牲畜中毒的事件常有报道[1]。为配合中毒病人的临床诊断与治疗,有必要建立全血中杀鼠迷的快速     

用高效液相色谱法快速测定甜菊糖甙

本文介绍了用高效液相色谱法分离测定甜菊糖甙的四种成分,测定了各成分的相对百分含量及甜菊饮料制品中各糖甙成分及糖类的含量,并做了精密度和回收率的验证。该法简便快速,效果良好。色谱条件为:μ-Bondapak NH_2往,柱前加Bondapak AX/Corasil预柱;乙腈:0.02M(NH_4))2 HPO_4水溶液=75:25作流动相,流速为2.0ml·min~(-1);示差折光检测。