高效液相色谱法测定血浆中莲心碱的浓度

采用高效液相色谱法（甲基莲心碱为内标）测定了血浆中莲心碱的浓度。以ＵｌｔｒａｓｐｈｅｒｅＳｉ为固定相、二氯甲烷－异丙醇－二乙胺（７５１５０．２,Ｖ／Ｖ）为流动相,检测波长为２８２ｎｍ。血样用氨－氯化铵缓冲液调ｐＨ１０后用乙醚提取。平均回收率９３．６％,ＲＳＤ为１．９％,最低检测浓度０．０２５ｍｇ／Ｌ。     

固相萃取-高效液相色谱法测定人血浆中的川芎嗪

建立了高效液相色谱测定人血浆中川芎嗪浓度的方法。色谱条件:分析柱为Luna C18(150 mm×4.6 mm i.d.,5 μ m),流动相为甲醇-乙腈-醋酸盐缓冲液(pH 5.0)(体积比为50∶8∶42),流速1.0 mL/min,柱温40 ℃,检测波长280 nm。 血浆样品预处理采用C8固相小柱萃取法。方法的线性范围为25～5000 μg/L,线性相关系数为0.9999。高、中、低浓度 的川芎嗪在标准血浆样品中的平均提取回收率为96.72％～100.90％,日内和日间相对标准偏差(RSD)小于8.64％,准确度 为99.59%~103.26%,检测限为10 μg/L。该方法的各项效能指标符合生物样品的分析要求,可用于川芎嗪制剂的人体药 代动力学研究。     

高效液相色谱法测定血浆中米非司酮

建立了测定血浆中米非司酮浓度的高效液相色谱分析方法。血浆样品以乙醚提取,常温下负压挥发至干,所得残渣用甲醇浸溶后进行测定。Spherisorb C18(250 mm×4.6 mmi.d.,5μm)为色谱柱,流动相为甲醇-乙腈-水(50 25 25)溶液,检测波长为302 nm,用外标法定量。结果表明,在0.05~10.00 mg.L-1范围内呈线性,检出限为0.01 mg.L-1;平均回收率为98.2%,日内、日间平均精密度分别为7.0%,8.3%。米非司酮血浆样品的萃后残渣于-20℃可保存至少7d。     

HPLC Determination of Xylazine in Equine Plasma by High Performance Liquid Chromatography

Abstract

A high performance liquid chromatographic (HPLC) method is described for the determination of xylazine in equine plasma. The drug and internal standard (pindolol) were separated on a 5 μm cyanopropyl-modified column (250 × 4.6 mm i.d.) using a buffer-acetonitrile mixture containing an ion pairing reagent. The drug and internal standard were isolated from plasma by liquid extraction into ethyl acetate. The method was validated over the concentration range 50–2000 ng/ml in plasma; the reproducibility, expressed as the mean co-efficient of variation was less than 5.0% for both between-day and within-day replicate determinations. The method was linear over the concentration range studied. No interferences were observed from endogenous plasma components and the limit of detection was 20 ng/ml. The method was successfully applied to the determination of xylazine in equine plasma in a crossover study design for pharmacokinetic measurements.     

高效液相色谱法测定血浆中舒必利浓度

讨论了测定舒必利血药浓度的反相高效液相色谱方法。选用美国Ｂｉｏ－Ｒａｄ７００型高效液相色谱仪,ＲＰ－３１８色谱柱,ＵＶ检测波长２９０ｎｍ,流动相为甲醇－水－冰醋酸（６０３０１）,内标物为胃复安。回收率为９７．９５％～９９．９６％,ＲＳＤ为２．６％～５．１％,最低检出浓度１．０ｍｇ／Ｌ,线性范围５～１００ｍｇ／Ｌ。测定３０例服药病人的血药浓度,得到了满意的结果。     

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－荧光检测法测定人血浆中匹伐他汀的含量

 Pitavastatin belongs to the class of coenzyme A reductase inhibitors. Very few methods of assaying pitavastatin from human plasma are available in literature. An analytical method is presented for the determination of the drug from human plasma making use of the fluorescent property of the drug. The drug is extracted from plasma using ethyl acetate under neutral condition and then analyzed by reversed-phase high performance liquid chromatography (HPLC) with fluorescence detection (λEx 245 nm; λEm 420 nm). Analysis of pitavastatin was carried out on a C18 HPLC column using a gradient flow of mobile phase (0.01 mol/L monobasic potassium phosphate (pH 3.20)-acetonitrile, 63∶37, v/v). Fluorescein isothiocyanate was used as internal standard. The dynamic range of assay was 3 to 50 ng/mL. The intraday precision was less than 10% and accuracy ranged from 95.2% to 112.6%. The same for interday check was less than 12% and 92.8% to 105.1%, respectively. The drug was found to be stable under the assay conditions. The developed method is simple, precise, accurate, and stable. This indicates that it can be applied to routine analysis of this drug in human subjects where there are large numbers of samples without the need of specialized instruments like column switching.     

高效液相色谱法测定血浆中表阿霉素浓度

报道了高效液相色谱法测定血浆中表阿霉素浓度的实验方法。采用μＢｏｎｄａｐａｋＣ＿（１８）色谱柱,正磷酸、甲醇、乙腈、异丙醇为流动相。荧光检测器检测,激发波长为４５０ｎｍ,发射波长为５３０ｎｍ。血浆经离心后,取血清,用甲醇沉淀蛋白。方法的平均相对回收率为９９．４％±４．６％,日内和日间平均ＲＳＤ小于５％和６％。最低检测限为３ｎｇ。本方法快速、准确,灵敏度高。     

高效液相色谱法测定人血浆中的辛伐他汀

 建立了高效液相色谱法监测人口服辛伐他汀药物后的血药浓度。血样用环己烷-二氯甲烷(体积比为3.5∶1)提取,以洛伐他汀为内标,在237nm波长下检测;色谱柱:LichrospherC18(200mm×4.6mmi.d.,5μm),流动相:乙腈-水(体积比为70∶30);流速:1.2mL/min。血药浓度在0.25～50.0μg/L范围内与峰面积和内标峰面积的比值之间线性关系良好,日内及日间相对标准偏差(n=5)分别低于7.94%和8.58%,回收率高于93.3%。方法灵敏、准确、快速,适用于药物动力学和药效学研究。     

Determination of Drugs in Blood Samples by High Performance Liquid Chromatography Using On-Line Sample Pretreatment Technique

The flow diagram of this on-line sample pretreatment system is shown in Fig. I.     

多功能柱净化-高效液相色谱法同时检测小麦中雪腐镰刀菌烯醇和脱氧雪腐镰刀菌烯醇

建立了小麦中雪腐镰刀菌烯醇（NIV）和脱氧雪腐镰刀菌烯醇（DON）的高效液相色谱同时检测方法。样品采用乙腈-水（体积比85：15）混合溶剂进行提取．通过多功能净化柱（MFC）进行一次性净化,以C18柱为分离柱,水-乙腈-甲醇（体积比90：5：5）混合溶剂为流动相进行高效液相色谱分离和检测。在小麦样品中,本方法在0．2～5μg／g添加范围内的凹收率为87％～99％;相对标准偏差为1．5％～8．3％;DON和NIV的检出限分别为0．12和0、16μg／g（5／N=3）。     

Identification of Apigenin Metabolites in Rat Liver Perfusate by Column Switching High Performance Liquid Chromatography/Electrospray Ionization Mass Spectrometry

Summary.  A selective column switching high performance liquid chromatographic method has been used for the simultaneous determination of apigenin and metabolites in rat liver perfusate. This new method clearly separated apigenin and the metabolites with high resolution. The structures of metabolites were proposed based on selective ion recording and full scan analysis by electrospray ionization mass spectrometry. Corresponding author. E-mail: basly@pharma.unilim.fr Received May 15, 2002; accepted (revised) September 13, 2002     

高效液相色谱柱切换技术在药代动力学与生物利用度研究中的应用

A review of the technique of HPLC column switching has been reported.It was used successifully in thestudy of pharmacokinetics and bioavailabily for seven drugs in our laboratory.It was detailed the conditionsand effective factors for determination of famotidine,mitoxantrone,gliquidone,difloxacin, ciprofloxascin,flucomzole and pseudoephedrine in blood.     

高效液相色谱法测定血浆中左亚叶酸钙的含量

建立了测定血浆中左亚叶酸钙含量的RPHPLC方法。采用DiamonsilC18色谱柱(150mm×4.6mm,5μm),乙腈50mmol/L磷酸氢二钾/磷酸二氢钾缓冲溶液(10∶90,V/V,用磷酸调pH至4.0)为流动相,用前经0.45μm的过滤膜,超声脱气,流速为1.0mL/min,紫外检测波长为290nm,柱温为35℃,进样量20μL。该方法最低检出限为0.2ng;线性范围为0.05～10mg/L,方法平均回收率在97.0%以上;日内及日间精密度的相对标准偏差分别小于4%和6%。该方法简单,快速,灵敏度高,重复性好。     

高效液相色谱法测定人血浆中甲磺酸培氟沙星浓度

建立了一种测定人血浆中甲磺酸培氟沙星的匠相液相色谱方法,用的是ＺｏｒｂａｘＯＤＳＣ＿（１８）柱和用三乙醇胺调节成ｐＨ为３．０的甲醇－０．０４ｍｏｌ／ＬＨ＿３ＰＯ＿４溶液（８０：２０,Ｖ／Ｖ）的流动相,检测在２７６ｎｍ处进行,流量为１ｍＬ／ｍｉｎ,线性范围是６．０１×１０￣（－８）～３．０１×１０￣（－５）ｍｏｌ／Ｌ（γ＝０．９９９８）,检测极限为６．０１×１０￣（－８）ｍｏｌ／Ｌ,平均回收率为９７．５７±３．０４％,日内与日间的ＣＶ分别为３．２９％和５．０８％。     

Determination of Cefaclor in Human Plasma by Reversed-Phase High-Performance Liquid Chromatography with UV Detection and Its Application to the Bioequivalence Studies

Abstract

A selective and sensitive reversed-phase high-performance liquid chromatography method was developed and validated for quantitation of cefaclor in human plasma using cefradine as an internal standard. Calibration curve was linear over range of 0.1–20 mg · L^?1. The intra- and inter-run relative standard deviations of the assay were less than 7%. The mean absolute recoveries determined at the concentrations of 0.3, 3.0, 8.0, and 15.0 mg · L^?1 were 69.9%, 69.9%, 77.1% and 72.0%, respectively. The analytical method established was proved to be specific, precise, sensitive, and suitable for applying in the pharmacokinetic and bioequivalence studies of cefaclor in human.     

高效液相色谱法测定肌苷注射液的含量

This paper describes an HPLC procedure for the assay of inosini in injection. The assay was carried outon a 250mm×4.6mm column with 5μm ODS using methanol-acetonitrile-water(40:10:50)as mobilephase,with UV detection at 248nm,The elution was performed at the flow rate of 1mL/min. This method issimple and accurate.     

反相高效液相色谱/电喷雾质谱法测定血浆中盐酸舍曲林

采用反相高效液相色谱-电喷雾质谱法(LC-ESI/MS)测定人体血浆中盐酸舍曲林。以盐酸丙咪嗪为内标,按内标法定量。血浆样品经pH 10.00碳酸钠溶液碱化,加入甲基叔丁基醚萃取,离心分离,取上清液吹干,用流动相溶解进样。色谱柱:RP-Extend-C18(150 mm×4.6 mm,5μm),柱温:40℃;流动相:pH 3.00的三氟乙酸溶液-甲醇(40∶60,V/V),流速0.6 mL/m in。质谱采用选择离子监控模式,检测离子的核质比(m/z)分别是281(丙咪嗪)和159(舍曲林)。舍曲林和丙咪嗪的保留时间分别是5.4 m in和3.8 m in;舍曲林标准曲线线性范围为1~80μg/L;检出限为1.0μg/L(S/N>10);日间、日内相对标准差均小于6.0%,相对回收率为90%~106%;提取回收率在75%~93%范围内。此法适合人体药代动力学的血浆样品的分析,结果准确、可靠。     

分子印迹柱-高效液相色谱法测定猪肉中磺胺嘧啶(英文)

建立了分子印迹柱-高效液相色谱法检测猪肉中磺胺嘧啶残留方法。制备了磺胺嘧啶的分子印迹柱,并优化了分子印迹柱的萃取条件。研究结果表明,在最佳萃取条件下,分子印迹柱-高效液相色谱法的加标回收率≥75.6%,相对标准偏差≤6.1%。分子印迹柱为固相萃取柱可以预浓缩与纯化猪肉样品中磺胺嘧啶。与氧化铝萃取柱比,分子印迹柱具有较好的重复性和萃取效率。本方法已成功用于实际猪肉样品中磺胺嘧啶含量的检测,结果满意。     

高效液相色谱法测定人血浆中总高半胱氨酸含量

建立了快速检测人血浆中总高半胱氨酸含量的高效液相色谱（HPLC）方法。采用反相HPLC分析前,以巯基特异性荧光试剂ABDF对血浆中巯基进行衍生．方法简便、灵敏、准确,无干扰峰影响。平均回收率为97．75％,日内和日间精密度分别为4．49％和9．79％。