固相萃取-高效液相色谱法测定枸杞中的类胡萝卜素

研究了固相萃取富集和预分离,高效液相色谱测定枸杞中的类胡萝卜素的方法;枸杞中的类胡萝卜素用WatersXterraTMRP18固相萃取小柱预分离,以WatersXterraTMRP18(3.9×150mm,5μm)液相色谱柱为固定相,甲醇 四氢呋喃(4 1)为流动相分离,用二极管矩阵检测器检测,检测波长为450nm。方法标准回收率为95%～103%。用该方法测定了几种枸杞样品中的类胡萝卜素。     

固相萃取-高效液相色谱法同时测定食品中4种合成色素

以可代替使用的水溶性合成色素-亮黑BN、固绿FCF、酸性红、酸性黄36为研究对象,建立了高效液相色谱同时测定食品中4种合成色素的方法。样品通过WAX固相萃取柱富集净化,10%氨化甲醇洗脱,采用C18色谱柱分离,以甲醇和10 mmol/L乙酸铵水溶液作为流动相梯度洗脱,外标法定量。通过固相萃取柱净化后,杂质对待测物的干扰明显降低,优化色谱条件下,4种色素在0.10~10.0 mg/L质量浓度范围内,线性良好,相关系数(r)≥0.9995。方法回收率为92.6%~101.8%,相对标准偏差(RSD)≤5.4%,方法检出限为0.01~0.04 mg/kg。该方法灵敏度高,准确可靠,适合食品中亮黑BN、固绿FCF、酸性红、酸性黄36的同时测定。     

固相萃取-高效液相色谱法测定地表水中的苯并三唑和苯并噻唑

建立了固相萃取-高效液相色谱分析地表水中苯并噻唑、苯并三唑、5-甲基-苯并三唑、5-氯-苯并三唑及5,6-二甲基-苯并三唑的方法。地表水样品采用HLB固相萃取柱富集净化后,在甲醇-水(55:45, v/v)流动相中用ZORBAX SB-C18色谱柱(250 mm×4.6 mm, 5 μm)分离,紫外检测,外标法定量。结果表明,5种目标化合物在0.064～80 mg/L范围内均呈良好的线性关系,线性相关系数均大于0.9999,仪器检出限为1.9～3.2 μg/L。空白自来水样中的加标回收率为87.8%～125.6%,相对标准偏差(n=3)为0.4%～9.4%。应用该方法测定了大连自来水及辽河入海口水样,在辽河入海口地表水中检出苯并噻唑、苯并三唑、5-甲基-苯并三唑、5-氯-苯并三唑。     

固相萃取高效液相色谱法快速测定红豆杉枝叶中的3种紫杉烷类化合物

研究了用固相萃取预分离高效液相色谱法测定红豆杉枝叶中紫杉醇、三尖杉宁碱和7 表紫杉醇的方法。其中,固相萃取使用了一种新型的PRP 6高分子树脂。红豆杉枝叶经干燥粉碎后用甲醇提取,提取液用PRP 6固相萃取小柱预分离,以V(乙腈)∶V(水)=45∶55为流动相,用C18色谱柱进行分离,紫外检测器227nm测定上述3种紫杉烷类化合物,该方法加标回收率为91%～98%。此法可以快速准确的测定不同红豆杉枝叶中上述3种紫杉烷类化合物。     

高效液相色谱法测定饲料用灌木中色素的研究

研究了用固相萃取预分离,高效液相色谱法测定饲料用的灌木中植物的色素的方法;饲料用的灌木样品中的色素用Sep Pak C18固相萃取小柱预分离和富集,以WatersNova Pak C18液相色谱柱为固定相,V(甲醇)∶V(异丙醇)=1∶1和水梯度洗脱为流动相分离。方法可同时测定叶黄素、α 胡萝卜素、β 胡萝卜素、叶绿素 a、叶绿素 b、紫黄质、新叶黄素(新黄质)等色素,方法标准回收率为94%～104%,相对标准偏差为1 9%～2 5%。已用于几种饲料用的植物色素的测定。     

用快速分离柱高效液相色谱法测定烟草中的几种酚

研究了用快速分离柱高效液相色谱法测定烟草样品中的苯酚、苯二酚和甲基苯酚. 烟草样品中的酚经水蒸汽蒸馏分离后用Waters Sep-Pak-C18固相萃取小柱富集, 以ZORBAX Stable Bound (4.6 mm i.d.×20 mm, 1.8 μm) 快速分离柱为固定相, 0.05 mol/L KH2PO4缓冲溶液-甲醇梯度为流动相, 几种主要酚在2.0 min 内可达到基线分离;该方法的相对标准偏差为2.1%～3.6%, 标准加入的回收率为88%～97%, 已用于几种烟草样品测定.     

固相萃取-高效液相色谱-可变波长检测法同时测定调味品中甜味剂和人工合成色素

建立了同时测定调味品中糖精钠和合成色素的固相萃取-高效液相色谱(SPE-HPLC)分析方法。样品经石油醚低温去除油脂,聚酰胺固相萃取柱净化和富集,然后进行HPLC分析。采用反相C₁₈色谱柱,以甲醇和0.02 mol/L醋酸铵为流动相进行梯度洗脱,使用可变波长分别在230、510、484和510 nm进行检测。实验结果表明:糖精钠与合成色素的分离效果良好,回收率为88.6%～97.1%,相对标准偏差小于5%;方法检出限均可达到0.05 mg/kg。该方法操作简单,结果准确可靠,重现性好,适用于大批量调味品中甜味剂和人工合成色素的同时检测。     

Screening of domperidone in wastewater by high performance liquid chromatography and solid phase extraction methods

Domperidone is a dopamine D₂ receptor antogonist, which has been used as antiemetic agent in human beings. It has been found in wastewater released by some pharmaceutical industries leading to the contamination of surface and ground water. Therefore, a sensitive, inexpensive and reproducible HPLC-SPE method was developed for the analysis of domperidone in the wastewater. The column used was Waters symmetry C₁₈ (15 cm × 0.46 mm, 5 μm). The mobile phase used was phosphate buffer (50 mM, pH 3.5) acetonitrile (80:20, v/v) at the flow rate 2.0 mL/min. The detection was achieved by using UV mode at 230 nm. The retention, separation and resolution factors were 2.63, 3.00 and 3.20, respectively. The percentage recovery of domperidone from wastewater was 95.0%. Celiprolol was used as the internal standard to access the percentage extraction of domperidone from wastewater.     

Selective determination of famotidine in human plasma by high performance liquid chromatography in alkaline media with solid phase extraction

A new method is described for the determination of famotidine by solid phase extraction from alkalinized human plasma followed by reversed phase (RP) HPLC in acetonitrile/alkaline buffer with molsidomine as an internal standard. Different acetonitrile/aqueous buffer mobile phases as well as various RP columns were used. Alkaline medium allowed the limit of quantitation to be lowered to 5 ng/mL of plasma as the famotidine gives more intense absorption at about 286 nm (at pH values higher than 7). Moreover, work in alkaline media and at this wavelength is highly selective as peaks corresponding to impurities present in most samples are well separated. A method using a mildly alkaline mobile phase (acetonitrile/10 mM phosphate with 10 mM 1‐heptanesulphonic acid, pH 7.5) was successfully used for determination of famotidine in human plasma in a pharmacokinetic study.     

分散固相萃取-高效液相色谱法快速测定果蔬中的6种保鲜剂残留量

建立了采用分散固相萃取-高效液相色谱同时测定果蔬中2,4-滴、噻苯咪唑、乙萘酚、邻苯基苯酚、二苯醚和联苯6种保鲜剂残留量的方法。样品经乙腈提取(同时加入氯化钠和无水硫酸镁),提取液经酸性氧化铝分散固相萃取净化,采用Agilent TC C18色谱柱(250 mm×4.6 mm, 5 μm),以甲醇-0.02 mol/L的磷酸二氢钾溶液(pH 6)作为流动相,流速1.0 mL/min,梯度洗脱,用紫外检测器检测,检测波长为235 nm,外标法峰面积定量。6种保鲜剂在0.5～20 mg/L范围内线性关系良好,相关系数均大于0.99; 6种保鲜剂在样品中添加1、2和10 mg/kg 3个浓度水平的回收率为84.2%～99.1% (n=6),相对标准偏差为1.67%～10.3%;方法的定量限为1 mg/kg。该法简便、准确,适用于果蔬中6种保鲜剂残留量的检测。     

分子印迹固相萃取-高效液相色谱法测定饲料中莱克多巴胺

以莱克多巴胺为模板分子,丙烯酰胺为功能单体,乙二醇二甲基丙烯酸酯为交联剂,合成了对莱克多巴胺具有高选择性的分子印迹聚合物。考察了甲醇、乙腈、丙酮和氯仿-甲醇与三乙胺构成致孔剂合成的聚合物性能及其形貌特征。通过正交试验优化的聚合反应配方为: 1.0 mmol莱克多巴胺,4.0 mmol丙烯酰胺,20.0 mmol乙二醇二甲基丙烯酸酯,6.0 mL乙腈-三乙胺(30:1, v/v), 50.0 mg偶氮二异丁腈。建立的基于分子印迹固相萃取-高效液相色谱测定饲料试样中莱克多巴胺的方法,在0.50～100 mg/L质量浓度范围内有良好的线性关系(r=0.9994);饲料试样中1.0、10及100 mg/kg 3个添加水平的莱克多巴胺平均回收率大于80%;批内、批间测定的相对标准偏差小于10%;检出限(信噪比为3)达到0.1 mg/kg。该方法灵敏、可靠,用于饲料等复杂基质中莱克多巴胺检测的效果优于相关标准分析方法。     

A novel molecularly imprinted polymer for simultaneous extraction and determination of sudan dyes by on-line solid phase extraction and high performance liquid chromatography

A novel molecularly imprinted polymer was synthesized with attapulgite employed as matrix, which is simple and time-saving. In this method, sudan I was chosen as template molecule, 2-vinylpyridine as functional monomer and ethylene glycol dimethacrylate as cross-linking agent, respectively. The imprinted polymer was characterized by the infrared spectroscopy and transmission electron microscopy. Then the selectivity experiments were performed on sudan dyes and the recognition coefficients for sudan I, sudan II, sudan III and sudan IV were 2.9, 1.9, 1.9 and 2.3, respectively. As the packing material of solid-phase extraction, the imprinted polymer has been applied to on-line concentration of the four sudan dyes in samples from Yellow River water, tomato sauce and sausage. The corresponding analytical methods to determine these sudan dyes have been developed. The limits of detection for these sudan dyes were in the range of 0.01–0.05 ng mL⁻¹ for Yellow River water, 1.0–3.0 ng g⁻¹ for tomato sauce and 0.8–3.0 ng g⁻¹ for sausage.     

Determination of halofuginone in bovine plasma by competing-ion high performance liquid chromatography after solid phase extraction

A high performance liquid chromatography (HPLC) method for the determination of the anticoccidial and antitheilerial drug halofuginone in bovine plasma was developed. Samples were diluted with acetic acid (10%, v/v) and cleaned up on a Bond Elut C8 column. The analyte was eluted from the extraction column and chromatographed by reversed-phase HPLC using decylamine as a competing-ion reagent. Detection was by UV at 243 nm. Recovery from plasma was 75%, and within-day and between-day coefficients of variation were 5.23 and 6.35% respectively. The specificity and sensitivity of this method (limit of detection in plasma, 1 ng/mL) were sufficiently high to enable us to characterize the time course of the drug in plasma after oral administration of therapeutic doses to cattle.     

离子交换固相萃取高效液相色谱联用法检测河豚鱼中的河豚毒素

优化建立了采用混合模式阳离子交换固相萃取柱代替传统的C18固相萃取柱进行前处理,联用高效液相色谱检测河豚鱼中河豚毒素的方法.样品经合1％乙酸的乙腈甲醇(3:1,V:V)溶液提取,混合模式阳离子交换固相萃取柱(MCX)净化,5％氨水/甲醇溶液洗脱,采用高效液相色谱-二极管阵列检测器(HPLC-PAD)测定,外标法定量.河...     

液液提取-固相萃取-气相色谱法测定牛肉中蝇毒磷残留量的研究

建立了液液提取-固相萃取-气相色谱火焰光度法(LLE-SPE-GC-FPD)测定牛肉中蝇毒磷的残留量.优化了气相色谱分离条件,研究了样品基质对蝇毒磷测定的影响,考察了Florisil固相萃取小柱和ODS固相萃取小柱的萃取效果,并选择乙酸乙酯为洗脱剂,考察了液-液提取和固相萃取的回收率.将该方法用于牛肉中蝇毒磷的测定,其检出限为0.02 μg/mL,回收率高于83%,相对标准偏差13.7%.使用气相色谱质谱仪(GC-MS)对样品中的蝇毒磷进行定性分析,其特征离子和相对丰度为362(100)、226(55)和210(40).     

固相萃取-反相高效液相色谱法同时测定饲料中的角黄素和虾青素

建立了一种同时测定饲料中角黄素和虾青素的固相萃取-高效液相色谱法（HPLC）。样品由乙腈提取,经LC-NH2固相萃取小柱净 化,洗脱剂为乙腈-甲苯（体积比为3∶1）,洗脱液被浓缩后进行HPLC分析,色谱柱为ZORBAX Eclipse XDB-C18柱(150 mm×4.6 mm,5 μ m),流动相为乙腈-甲醇（体积比为95∶5）,流速1.0 mL/min,采用二极管阵列检测器检测,检测波长为474 nm;外标法定量。角黄素和 虾青素的线性范围分别为1.0～30.0 mg/L和1.0～20.0 mg/L,相关系数分别为0.9990和0.9991,回收率为90%～101%,相对标准偏差为 0.62%～3.68%,检出限分别为0.84和0.60 mg/L。该方法简便、快速、准确,可用于饲料中角黄素和虾青素的同时测定。     

Determination of fluoroquinolones in edible animal tissue samples by high performance liquid chromatography after solid phase extraction

In the present work, a rapid, accurate, and sensitive method has been developed for the quantitative determination of five fluoroquinolones (enoxacin, ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin) in edible animal tissues (muscle tissue, liver, kidney, and eggs). The separation was accomplished on an Inertsil (250 x 4 mm) C8, 5 microm, analytical column, at ambient temperature within 15 min. The mobile phase consisted of a mixture of citric acid (0.4 mol L(-1))-CH3OH-CH3CN (87:9:4% v/v). UV detection at 275 nm yielded the following limits of detection: 100 pg per 20 microL injected volume for enoxacin, norfloxacin, and ciprofloxacin, 20 pg for ofloxacin, and 200 pg for enrofloxacin. Peaks in real samples were identified by means of a photodiode array detector. The method was validated in terms of intra-day (n = 8) and inter-day (n = 8) precision and accuracy. Tissue samples were purified from endogenous interference by solid-phase extraction using Oasis HLB cartridges. The solid-phase extraction protocol was optimized in terms of retention and elution. Recovery rates at fortification levels of 40, 60, and 80 ng/g ranged from 82.5% to 111.1%. The applicability of the method was examined using real samples from a chicken treated orally with the five studied fluoroquinolones.     

固相萃取-高效液相色谱法同时测定牛奶中22种磺胺类兽药残留

建立了一种基于固相萃取技术同时测定牛奶中22种磺胺类兽药残留的高效液相色谱分析方法.样品经乙腈-甲酸混合溶液提取,乙腈饱和的正己烷除酯后,HLB固相萃取柱净化,以甲醇-2 mmol/L乙酸铵(含0.2％乙酸)为流动相进行梯度洗脱,XBridge C18色谱柱进行分离,采用光电二极管阵列检测器检测,外标法定量.磺胺类化合...     

固相萃取-高效液相色谱法测定烟草中的两种多羟基吡嗪异构体

用固相萃取-高效液相色谱-二极管阵列检测法建立了测定烟草中两种多羟基吡嗪异构体的方法.烟草中的2-(1′,2′,3′,4′-四羟基丁基)-5-(2″,3″,4″-三羟基丁基)-吡嗪(2,5-DOF)和2-(1′,2′,3′,4′-四羟基丁基)-6-(2″,3″,4″-三羟基丁基)-吡嗪(2,6-DOF)用甲醇索氏萃取2h后,提取液用Waters Sep-Park-C18固相萃取小柱预分离,选择Waters carbohydrate analysis(3.9 mm×300 mm)色谱柱(NH2柱),V(乙腈)∶V(水)=80∶20为流动相,流速:1.0 mL/min,烟草中的2,5-DOF及2,6-DOF达到基线分离.两种异构体的标准曲线的线性回归系数均大于0.9996,线性范围为0.5～100 μg/mL;标准回收率分别为98%和104%;相对标准偏差均小于3%;检出限为0.2 μg/mL.用该方法测定了不同卷烟中的2,6-DOF和2,5-DOF两种异构体.     

Purification and determination of plant hormones auxin and abscisic acid using solid phase extraction and two-dimensional high performance liquid chromatography

A method for separation and purification of plant hormones auxin and abscisic acid based on mixed mode reversed-phase anion-exchange solid phase extraction and two-dimensional HPLC was developed. Two-dimensional HPLC in "heart cutting" mode was very efficient in the purification of these two hormones. Its purification power is high enough to allow reliable on-line quantification of both hormones even with non-selective detectors.