固相萃取-LC/MS分析尿液中丁丙诺啡

目的:建立固相萃取-LC/MS分析尿液中丁丙诺啡方法。方法:在含有丁丙诺啡的尿液中,加入β-葡萄糖醛酸酶溶液,50℃水解2小时,加入内标奋乃静,加pH10.8缓冲溶液,用401有机担体作吸附剂,用三氯甲烷作洗脱剂固相萃取,洗脱液于50℃水浴中氮气流下吹干,残余物用流动相溶解后LC-MS分析。结果:方法的线性范围为0.2～100.0μg·L~(-1),检出限为0.1μg·L~(-1)。结论:该方法灵敏度高,可用于涉毒案件尿液中丁丙诺啡的分析。     

高效液相色谱法测定毛豆中吡虫啉残留量

采用高效液相色谱法测定毛豆中吡虫啉农药残留。试样用二氯甲烷超声波提取,中性氧化铝柱净化,石油醚去除脂类杂质,以0.2%冰乙酸水溶液-乙腈(70:30,体积比)为流动相,配备Agilent TC-c18柱、高效液相色谱紫外检测器检测(HPLC-UV),外标法定量。实验表明,毛豆样品中吡虫啉添加回收率为84.0%~102.8%,相对标准偏差(n=6)为6.8%~10.9%,样品中吡虫啉最低检测浓度为0.003 mg/kg。     

Specific Proline and Hydroxyproline Detection Method by Post-column Derivatization for High-performance Liquid Chromatography

A specific detection method for hydroxyproline by post-column derivatization with 7-chloro-4-nitrobenzo-2-oxa-l,3-diazole was developed after chiral resolution by ligand-exchange chromatography. The addition of ethylenediaminetetraacetic acid to the reaction mixture was effective to achieve the post-column reaction. The calibration curve for trans-4-hydroxy-L-proline shows linearity from 7.6 pmol up to 7600 pmol.     

测定浮游植物中色素的高效液相色谱与二极管阵列分光光度计联用的方法

建立了高效液相色谱与二极管阵列分光光度计联用分析浮游植物中色素的方法.采用90%的丙酮提取藻类中的类胡萝卜素和叶绿素后在反相C18柱上分离,流动相选用甲醇/醋酸铵/丙酮,流速为2.0 mL*min-1.用可见光检测器检测,波长为440 nm.在线的二极管阵列检测器对色素峰的扫描(400～700 nm)得到各色素峰的吸收光谱的结果显示,保留时间相同的色素峰,吸收光谱可能不同.根据色素峰吸收的光谱特性确定色素的种类,可以避免色素峰保留时间相同而造成的判断误差,从而提高了分辨的准确性.     

Xterra RP18柱高效液相色谱法快速分离测定氨基酸

建立了一种用XterraRP1 8色谱柱快速分离测定水解氨基酸的方法。所采用的色谱条件是 :WatersAlliance系统 ,柱温 5 6℃ ,流速 1 .8ml/min ,检测波长 2 4 8nm ,梯度分离 ,运行周期 2 5min,柱反压低于 2 0 0 0Psi。在 1 7.5min内分离了包括AMQ、NH3 和牛磺酸在内的 2 1种氨基化合物 ,适应于复合氨基酸注射液、含牛磺酸的氨基酸口服液及水解氨基酸样品的分析测定     

离子交换高效液相层析法测定腺苷酸环化酶活性

用离子交换高效液相层析（ＨＰＬＣ）分离并同步测定脑组织腺苷酸环化酶（ＡＣ）反应生成的ｃＡＭＰ,从而直接测定ＡＣ活性。１００℃加热１ｍｉｎ终止ＡＣ反应后,混合物在０℃放置２ｈ。在此期间,反应体系中残留的ＡＴＰ水解酶将反应混合物中大部分剩余的ＡＴＰ水解除去。用二氯甲烷抽提除去罂粟碱等干扰物质,使混合物中的ｃＡＭＰ同蓁物质在Ｓｈｉｍ－Ｐａｋ ＷＡＸ－１阴离子交换ＨＰＬＣ术上基线分离,并可定量测定,用此方     

SPE-HPLC法快速检测发酵液中紫杉醇的含量

针对红豆杉内生真菌发酵液中紫杉醇的含量测定进行探讨,以建立快速高效低耗的检测方法.采用C_(18)固相萃取柱对紫杉醇进行吸附,用不同浓度的甲醇-乙酸铵和甲醇分别作为洗脱剂对其进行洗脱,比较两者的洗脱效果,洗脱液用HPLC进行检测;色谱条件为:流动相甲醇(v):水(v):乙腈(v)=20: 45: 35,流速:0.70 ml/min,检测波长:227 nm.结果表明,浓度为80%的甲醇溶液洗脱效果较好,紫杉醇的回收率为87.6%.     

蜂王浆中抗生素残留物质氯霉素的含量测定

本文对蜂王浆中抗生素残留物质氯霉素(Chloramphenicol)的检测方法进行了探讨,建立了氯霉素残留的HPLC定量方法。样品采用液液分配和固相萃取法(SPE)进行纯化。氯霉素在0.1～10μg/mL间呈良好的线形关系,加样回收率为80.6～90.3%,RSD为3.48～5.63%。该方法稳定可靠,为蜂王浆产品中氯霉素残留的检测提供了依据。     

Separation and Quantification of Abscisic Acid and its Metabolites by High-performance Liquid Chromatography

A technique for the separation and quantitative estimation ofabscisic acid and its metabolic products, phaseic acid and dihydrophaseicacid by high performance liquid chromatography (HPLC) is described.The efficiency of two HPLC columns, LiChrosorb RP-18 and LiChrosorbNH₂ is compared. The method has been tested using extracts fromtomato plants and some of the results are presented. Abscisic acid, dihydrophaseic acid, phaseic acid, chromatography, tomato, Lycopersicon esculentum, Mill     

高效液相色谱法直接测定当归中阿魏酸的含量

建立了一种高效液相色谱法直接测定当归中阿魏酸的含量。色谱柱为Shim-pack CLC-ODS(6.0 mm i.d×150 mm,5μm),流动相为甲醇—1.0%冰醋酸水溶液(体积比为25∶75),流速为1.0 mL/min,检测波长为313 nm。研究结果表明:阿魏酸的线性范围为1.0~10.0 mg/L,回归方程为A=13.352 8C 0.013 6(r=0.998 5),最小检测限为10 ng,加样平均回收率为94.67%,相对标准偏差(RSD)为1.57%。方法操作简便、快速、灵敏、准确。     

高效液相色谱法测定辣椒素

用95%醋酸钠饱和乙醇溶液抽提辣椒树脂油中的辣椒素,经高效液相色谱(HPLC)分离,在紫外波长280 nm处测定。用此法分析测得福建特产"小米椒"的辣椒素含量为10.38%。     

Resting Eggs as New Biosorbent for Preconcentration of Trace Elements in Various Samples Prior to Their Determination by FAAS

In this study, the resting eggs of aquatic creatures living in freshwater (Daphnia, Cladocera, Crustacean) ecosystems were used as a novel biosorbent extractant for synchronous preconcentration of trace Cd(II), Co(II), Cu(II), Mn(II), and Ni(II) previous to measurement by flame atomic absorpiton spectrometry (FAAS). Using column procedures, optimization studies were conducted to realize the effective adsorption of the analyte ions such as the solution pH, amount of the biosorbent, volume of the sample, interfering ions, etc. A high preconcentration factor of 67 and low relative standard deflection of ≤4.1 % (n?=?8) were obtained. The invention constrains based on the 3 s/b criterion were 2.4 for Cd(II), 41.4 for Co(II), 4.2 for Cu(II), 3.0 for Mn(II), and 9.6 μg L^?1 for Ni(II). The accuracy of the method was verified by analysis of a certified standard reference material. The used procedure was applied to the definition of the analytes in diverse environmental samples with convincing results. Consequently, the resting eggs of Daphnia can be used as a biosorbent for preconcentration and biosorption studies.     

高效液相色谱法测定大麦虫磷脂酰胆碱含量

建立高效液相色谱法测定大麦虫体内磷脂酰胆碱含量的方法。样品经甲醇提取、净化后,经高效液相色谱分析。采用外标法定量,磷脂酸胆碱标准溶液质量浓度在250～2 000 μg/mL范围内呈良好的线性相关,相关系数为0.999 6,样品加标回收率在97%～109%之间,相对标准偏差小于2.4%。对不同生长阶段大麦虫体内磷脂酰胆碱含量测定结果表明,大麦虫体内卵磷脂含量随个体重量的变化符合二项式曲线的变化规律,相关系数R2=0.865(P＜0.01)。     

Determination of Carboxylic Acids in Wines by Liquid Ion-Exclusion Chromatography

The chromatographic behavior of aromatic and aliphatic acids was studied using an ion-exclusive column. The conditions were determined under which the separation of the acids by single-column ion-exclusion chromatography with UV detection was the most selective and efficient. The method developed was employed for determining the content of carboxylic acids in wines.     

高效液相色谱法测定血浆中同型半胱氨酸

建立了一种高效液相色谱-库仑阵列电化学测定血浆中同型半胱氨酸的方法。采用3-2-羧乙基膦作为还原剂还原巯基间形成的二硫键,用0.1 mol.L-1HC lO4来沉淀血浆蛋白,离心取上清,进样分析。在0.40~50.00μmol.L-1范围内,线性关系良好。加标平均回收率是98.43%,RSD%是4.35%。该方法简单、快速、灵敏。     

一种根系分泌物中有机酸的前处理和高效液相色谱检测方法

改进了根系分泌有机酸的前处理和高效液相色谱检测方法.将DEAE纤维素层析法直接用于根系分泌物中有机酸的富集浓缩,并与旋转蒸发浓缩的回收率进行了比较.结果表明,DEAE纤维素柱层析有较高的回收率,可用于根系分泌物中有机酸的富集浓缩,特别适用于大批量样品的前处理.确定了反向高效液相色谱同时检测草酸、酒石酸、马来酸、苹果酸、乙酸、柠檬酸、琥珀酸等7种有机酸的条件.玉米根系分泌物样品中可检出苹果酸等5种有机酸.     

Lipophilicity Determination of Highly Lipophilic Compounds by Liquid Chromatography

Different experimental strategies using short columns in both conventional liquid chromatography (HPLC) and ultra‐high pressure liquid chromatography (UHPLC) were evaluated to allow, for the first time with these techniques, the lipophilicity determination of compounds with log P>5. Various organic modifiers, stationary phases, and elution modes were tested on 14 rigid compounds with a CLogP between 5 and 8, and 38 compounds with log P_oct from 0 to 5. The best results in HPLC were obtained with the 20‐mm Discovery ^® RP Amide C16 stationary phase in isocratic mode using MeOH as organic modifier. To improve analysis time, the UHPLC approach was then evaluated. Consequently, a generic method was developed with a 30‐mm Acquity BEH Shield RP18 column in gradient mode using MeOH as organic modifier, allowing a fourfold gain of time compared to the HPLC method, for the highly lipophilic compounds tested. Finally, the most rapid and accurate results were obtained with a 10‐mm Hypersil^TM GOLD Javelin HTS stationary phase in UHPLC, enabling an eightfold gain of time compared to the HPLC method.     

高效液相色谱法测定超滤后血浆中的谷氨酰胺

用高效液相色谱法测定超滤后血浆中的谷氨酰胺, 平均回收率为96.75%, 在130～1300μmol/L范围内呈线性关系(r=0.9906), 健康人正常值男性为(694.97±102.31)μmol/L, 女性为(623.79±99.27)μmol/L, 男女间值有显著差别(P＜0.05)该分析方法简单、迅速, 可用于外科肠道内营养的监测和对肠粘膜结构与功能的研究.