高效液相色谱法测定茶饮料中的咖啡因

本文探讨了用高效液相色谱法测定茶饮料中的咖啡因的最佳波长、流动相、柱温、流速等条件。获得的最佳检测条件为：波长273nm,流动相乙腈∶水=20∶80,柱温20℃,流动相流速1m L/min。在0~200μg/m L的浓度范围内线性关系良好,加标回收率为99.69%。建立的方法能够准确的测定茶饮料中的咖啡因含量。

反相高效液相色谱法测定不同产地丹参中丹参素的含量

丹参是一种双子叶唇形科植物丹参的根及根茎。近年来，广泛应用于心血管疾病的治疗，其具有降血压、降血脂、抗血栓、增加冠状动脉血流量及改善血液循环等作用。其主要功能成分是丹参素［1］。本实验采用反相高效液相色谱法测定丹参中丹参素的含量，并比较安徽、江苏、河北、湖北四个不同产地中两年生、三年生及五年生的丹参中丹参素的含量。

反相高效液相色谱法测定三唑仑的血药浓度

目的建立一种快速、准确的高效液相色谱法测定三唑仑的血药浓度。方法采用Kromasil C18柱（5um，4．6×250）；流动相为甲醇-水（65：35）；流速：1mVmin；柱温：40℃；检测波长：220nm；灵敏度：1．00AUFS。结果三唑仑在20～18300ng/ml范围内线性良好，日内RSD为4％～5％：日间RSD为3％～9％。绝对回收率为：88．72％～92．45％；方法回收率为：95．73％～103．95％。结论该方法简便、快速、准确、灵敏度高，可用于三唑仑的血药浓度测定。

高效液相色谱法测定地高辛片的含量

目的:建立地高辛片的含量测定方法。方法:采用高效液相色谱法(HPLC法)测定,以HypersilC18柱(150mm×4.6mm,5μm)为色谱柱,水-乙腈(36∶64)为流动相,流速为1mL/min;检测波长为230nm。结果:地高辛浓度线性范围为10～75μg/mL(r=0.9999),方法平均回收率为99.6%,RSD为0.75%。结论:HPLC法灵敏,结果准确,重现性好,可用于该产品质量控制。

液液萃取—高效液相色谱法测定地表水中硝基氯苯类化合物的尝试

硝基氯苯类化合物是被广泛应用于农药、医药和合成材料等行业的对人体有一定毒性的物质,对硝基氯苯和2,4-二硝基氯苯被多国列为优控污染物。针对这两种化合物,普遍采用气相色谱法进行分析,但由于该类化合物的热不稳定性,给气相色谱法的定量分析带来困难。尝试利用高效液相色谱测定地表水中的对硝基氯苯和2,4-二硝基氯苯,出峰效果良好,标准曲线为y=3.228 1x+0.138 3(R^2=0.999 9)和y=2.262 3x-0.077 6(R^2=0.999 9)。对实验条件进行优化,确定最佳检测波长、流动相配比和流速。

液液萃取—高效液相色谱法测定地表水中阿特拉津和甲萘威

本文对液液萃取-高效液相色谱法同时测定地表水中的阿特拉津(Atrazine)和甲萘威(Carbaryl)的过程进行了较为详细的阐述,并对样品预处理条件(萃取溶剂、样品预处理p H值)和色谱分析条件(色谱吸收波长、流动相、柱温和流速)进行了优化,旨在提高地表水特定项目的分析效率和改进其分析技术。

高效液相色谱法测定十全大补酒中芍药苷的含量

目的:建立十全大补酒中芍药苷的含量测定方法.方法:采用反相高效液相色谱法,Shim-peck CLC-ODS色谱柱;流动相为甲醇-水(34:66);检测波长为230 nm.结果:此方法芍药苷在0.5～1.75 μg线性关系良好,r=0.999 7;回收率为100.7%,RSD为0.3%.结论:方法简便、定量准确、重复性好,可用于十全大补酒的质量控制.

高效液相色谱法测定感康中扑热息痛含量

感康是由扑热息痛、金刚烷胺、人工牛黄、咖啡因等组成的复方制剂。有关复方制剂中扑热息痛的含量测定方法较多,常用亚硝酸钠法,方法繁琐,近年来利用多波长和高效液相色谱法测定扑热息痛含量的报导较多。作者参考有关文献采用了高效液相色谱法测定扑热息痛,操作简便,结果较好。1 仪器与试药高效液相色谱仪:日本岛津 Lc～4A。

高效液相色谱法测定肋柱花四味汤散中盐酸小檗碱的含量

目的利用高效液相色谱法测定肋柱花四味汤散中盐酸小檗碱的含量。方法采用C18柱,流动相为乙腈-0.05mol·L-1磷酸二氢钾(用磷酸调节pH至3)(30∶70);流速1.0ml·min-1;检测波长346nm;柱温25℃。结果盐酸小檗碱在0.03914～0.3914μg范围内线性关系良好(r=0.9999),平均加样回收率为99.8%,RSD为2.62%。结论该法简便、准确、可靠、重复性好,可用于肋柱花四味汤散的质量控制。

加替沙星注射液的研制和质量控制

目的 :探讨加替沙星注射液的处方、制备工艺及质量控制方法。方法 :以盐酸、氢氧化钠为 pH调节剂及氯化钠为等渗调节剂制备加替沙星注射液 ;采用高效液相色谱法测定本品的含量。结果 :制备的加替沙星注射液 (pH 5 .0 )在高温 (80°C)、光照(3 60 0lx) 1 0d及室温留样考察 2 4mo ,物理及化学性质稳定。结论 :处方及工艺经中试放大制备的注射液性质稳定 ;质量控制方法准确可靠 ;可满足临床用药要求。

尿液中羟基红花黄色素A的含量测定

目的:建立高效液相色谱法用于测定人尿液中羟基红花黄色素A的含量。方法:采用乙腈∶0.2%磷酸水溶液(20∶80 v/v)为流动相,流速为1 mL/min,检测波长为400 nm。结果:羟基红花黄色素A的线性范围为0.58～57.69μg/mL,羟基红花黄色素A在尿中3个浓度的绝对回收率分别平均为100.3%、100.8%、100.9%。结论:本方法简单快速,准确灵敏,重现性好,适用于羟基红花黄色素A的尿中药物浓度测定。

高效液相色谱法测定大鼠血浆中瑞格列奈浓度及其药动学

目的:建立大鼠血浆中瑞格列奈浓度的HPIC测定方法,并研究瑞格列奈在大鼠体内药物动力学行为。方法:血浆样品经酸化后,加入内标物,用醋酸乙酯提取,色谱柱为Kromasil C_(18)(150mm×4.6 mm,5 μm),流动相为0.1mol·L^(-1)柠檬酸-醋酸钠缓冲液(pH 4.0)-甲醇(27:73),流速为1.0mL·min^(-1),紫外检测波长243 nm,进样量20μL。测定了12只受试大鼠单剂量灌服瑞格列奈4 mg后血药浓度-时间过程。结果:最低检测为2.5 ng·mL^(-1),相对回收率平均为97.85%,日间和日内的变异系数小于5,线性范围为2.5～100 ng·mL^(-1),符合生物样品分析的要求。受试大鼠灌服瑞格列奈片4 mg后,估算的末端相半衰期(0.83±0.16)h,t_(max)(0.75±0.41)h,C_(max)(48.6±15.7)ng·mL^(-1)。结论:建立的HPLC方法适合于血浆中瑞格列奈浓度的测定及药动学研究。

高效液相色谱法测定糕点中富马酸二甲酯

目的研究糕点中富马酸二甲酯快速、准确、简单的高效液相色谱法测定方法。方法样品经甲醇提取后,用超纯水定容,选用Eclipse XDB-C18分离柱,流动相为甲醇:水(35:65)(V:V)。以保留时间定性,峰面积定量。结果回收率在91.86%～104.8%之间;检出限为0.24mg/L;相关系数r>0.9998,结论该方法快速、简单、准确,可用于糕点中富马酸二甲酯测定。

Determination of 13 preservatives in cosmetics by high performance liquid chromatography and verification by mass spectrometry

A method using high performance liquid chromatography(HPLC)was developed for the s imultaneous determination of 13 preservatives(levulinic acid,p-hydroxyacetophenone,raspberry ketone,p-anisic acid,caprylhydroxamic acid,hydroxyethoxyphenyl butanone,methylisothiazolinone,phenoxyethanol,b e n z oic acid,methylparaben,chlorphenesin,dehydroacetic acid,and 5-bromo-5-nitro-1,3-dioxane)in cosmetics.Different types of samples were ultrasonically extracted by methanol,then the separation of 13 preservatives was carried out on a column of Agilent ZORBAX Eclipse XDB-C18(250 mm×4.6 mm,5μm)by gradient elution at a flow rate of 1.0 mL/min,using 0.1%phosphoric acid solution and acetonitrile as mobile phases.The column temperature was 30℃,and the detection was completed by a diode array detector with the wavelengths at 275,230 and 210 nm.Suspected positive samples were further confirmed by liquid chromatography-tandem mass spectrometry or gas chromatography-mass spectrometry.The linear regression analysis data shows good linearity for 13 preservatives in the respective mass concentration range,with their correlation coefficients(r)greater than 0.9998.The limits of detection(LODs)and limits of quantitation(LOQs)of the method are in the ranges of 0.4-100.0 mg/kg and 1.2-250.0 mg/kg,respectively.At three spiked levels,the average recoveries for 13 target compounds in three kinds of matrix samples are within 84.0%-115.4%,and the relative standard deviations(RSD)are within 0.5%-4.8%(n=6).This method is convenient,efficient,and precise,which can be used for qualitative and quantitative analysis of common preservatives in daily cosmetics.

Simultaneous determination of 27 preservatives in toothpaste by high-performance liquid chromatography

A method of high-performance liquid chromatography(HPLC)was established for simultaneous determination of 27 preservatives in toothpaste.Toothpaste samples were extracted with 50%aqueous methanol solution,ultrasonicated and then filtered.The target compounds were separated on a C_(18) column(250 mm×4.6μm,5μm)with the mobile phase consisting of acetonitrile and aqueous phosphoric acid solution,the column temperature was 30℃,the sample volume was 10μL,the flow rate was 1 mL/min,and diode array detector was used.Under the optimal experimental conditions,good linear relationship was obtained and the correlation coefficient(R^(2))was greater than 0.9995.This method was accurate and sensitive,which was suitable for the qualitative and quantitative analysis of 27 preservatives in toothpaste.

槐角丸中槲皮素和没食子酸含量的HPLC测定

Objective:To determine the contents of the four efficacious elements(quercetin;ellagic acid) in Huaijiao Wan by RP-HPLC.Method:High Performance Liquid Chromatograph is employed with a Column of Diamonsil ODS-C18(4.6mm×250mm,5.0μm) and a mobile phase of MeOH-H2O-HAc(2∶3∶0.15),the detection wavelength being 270 nm and the column temperature being 300C.Result:Nice linear relation exists when,quercetin is within 0.2048-1.229μg and ellagic acid within 0.5325-3.192 μg.The R value of each group is 0.9991 and 0.9998.The average rate of recovery of the two groups is between 98.0% and 99.1%.The RSD of each group is 1.02% and 0.40%(n=5).Conclusion:With this method,the two efficacious elements could be determined simultaneously.And for its convenience,nicety,high sensitivity and fidelity,it is applicable to the quality examination of Huaijiao products and to manufacturers’ control of quality.

Extraction Condition Optimization and Identification of Phenols from Lonicerae flos

Polyphenols were obtained from the natural dried Lonicerae flos by ultrasound-assisted extraction with ethanol as the solvent.Single factor experiment and response surface methodology were employed to optimize the extraction conditions.Ultra-performance liquid chromatrography(UPLC)-tandem mass spectrometry(MS/MS)was employed to identify polyphenols based on the plant widely targeted metabolomics database in a qualitative and quantitative manner.The results showed that the optimal extraction conditions for total phenols from Lonicerae flos were ultrasound-assisted extraction with a solid-to-liquid ratio of 10∶1 g/mL and 57%ethanol at 70 W and 60°C for 11 min.The yield of total phenols extracted under the optimal conditions reached 71.08 mg/g.The phenols in Lonicerae flos were mainly chlorogenic acid isomers,and the flavonoids were mainly nobiletin,galuteolin,and homoarbutin.

HPLC法测定银杏叶片中萜类内酯的含量

目的建立高效液相色谱法测定银杏叶片中银杏萜类内酯的含量测定方法。方法采用Agilent Zob-ax SB-C18柱(150mm×4.6mm,5μm),以甲醇-四氢呋喃-水(20∶8∶72)为流动相,蒸发光散射检测器。结果银杏内酯A在2.10μg-10.50μg范围内呈良好的线性关系(r=0.9997),平均回收率为96.67%;银杏内酯C在2.04μg-10.20μg范围内呈良好的钱性关系(r=0.9998),平均回收率为100.30%。结论该方法简便、快速、结果准确,适用于银杏叶片的质量控制。

Stability of Baicalin Aqueous Solution by Validated RP-HPLC

Aim In the present study a RP-HPLC method was developed and validated toinvestigate the stability of baicalin aqueous solution. Methods The influences of temperature and pHon the stability of baicalin aqueous solution were investigated by classic homoiothermicacceleration test, and the pH for the most stable solution was determined. Results The time whenbaicalin suffered 10% loss was found to be 18.1 h, and the degradation activation energy of baicalinwas 79.1 kJ·moL^(-1) . The pH at which baicalin is most stable is 4.28. Conclusion The temperatureshould be kept at a lower level and the pH should be adjusted to near that for the most stablesolution in the production of baicalin preparations.

Enantioseparation of Zolmitriptan by HPLC

Aim To establish a HPLC method for the separation of the enantiomers of zolmitriptan. Methods The separations were performed on Chiralcel OJ column with hexane-ethanol-diethylamine（85：15：0.2） as mobile phase at a flow rate of 0.8 mL·min^-1 and detecttion wavelength of 227 nm at 35 ℃. Several related parameters for separation were studied. Results Baseline separation （Rs 〉 1.5） was easily obtained in the case, and the R-isomer impurity in zolmitriptan was determined. Conclusion The method developed in this study has been successfully applied for quality-control purposes.