MonacolinK的高效液相色谱法研究

对高认相色谱法测定发酵液中ＭｏｎａｃｏｌｉｎＫ的含量进行了研究,找出了最佳流速,劝相配比等条件,测定其重现性,等指标证明此方法具有快速准确的特点。     

高效液相色谱法制备甲基对硫磷农药标准品的研究

ＨＰＬＣ技术由于具有快速、灵敏、准确、分辨率高、重复性好等优点，已广泛地应用于在药分析及残留分析。但采用ＨＰＬＣ技术制各在药标准品还未见报道，首次采用反相ＨＰＬＣ技术，以Ｃ１８作固定相，用甲醇—水（７６：２４）作流动相，分离工业原油制各甲基对硫磷农药标准品，所得标准品纯度在９９％以上。并考察了流动相组成、流速、进样体积、进样量等分离甲基对硫磷原油色谱分辨率、峰形及所收集产品纯度的影响，找出了纯化甲基对硫磷样品的最佳条件。     

霍夫曼降解反应制备3,5-二甲基苯胺及反应动力学研究

文章以均三甲苯为原料,经过氧化、胺化和降解反应得到3,5-二甲基苯胺,重点研究了由3,5-二甲基苯甲酰胺霍夫曼降解制备3,5-二甲基苯胺的反应及由N-溴代-3,5-二甲基苯甲酰胺制备3,5-二甲基苯胺反应的动力学。结果表明,在降解反应中,当物料比n(3,5-二甲基苯甲酰胺)∶n(NaOH)∶n(Br2)=1∶12.12∶4.24,重排反应温度为0℃,水解温度为90~100℃,水解时间为1h,3,5-二甲基苯胺的收率较高,为45%;动力学反应活化能(Ea)为1.04×105J/mol。     

高效液相色谱法同时测定脂溶性维生素

本实验利用高级液相色谱法（ＨＰＬＣ）同时测定强化乳粉中的脂溶性维生素ＶＡ、ＶＤ、ＶＥ。使用的色谱条件：μ─ＢｏｏｄｓｐａｋＣ１８柱为色谱分析柱（规格３．９×３００ｍｍ），以甲醇—水《Ｖ／Ｖ９９：１）为流动相，检测波长设置在２８０ｎｍ，样品制备采用直接用碱（４０％）进行皂化。实验测得的平均回收率ＶＡ９７．４６％，ＶＤ９８．０６％，ＶＥ１０２．４４％，变异系数分别为ＶＡ５．１３％、ＶＤ４．８８％、ＶＥ５．６９％。     

高效液相色谱法测定二氯喹啉酸

应用反相离子对高效液相色谱法对二氯喹啉酸原药进行了定量测定, 获得满意结果,方法的标准偏差是０．３１,变易系数为０．３８,回收率为９９ ．１１ ％ ～１０２ ．６ ％ 。     

高效液相色谱法测定山楂中有机酸的研究

本文研究了山楂中有机酸的高效液相色谱分析法.该方法对六种有机酸的平均回收率为87.9%～108.1%,变异系数为3.1%～10.3%.分析结果表明山楂中含有六种以上有机酸,含量以柠檬酸为最高,其次是苹果酸、草酸、琥珀酸和抗坏血酸,富马酸含量较少,此外还含有四种未定性的未知酸.     

大枣多糖的单糖组成的高效液相色谱法研究

用高效液相色谱法研究了大枣多糖的单糖组成。大枣中性多糖的组成单糖为：Ｌ－阿拉伯糖、Ｄ－半乳糖和Ｄ－葡萄糖。酸性我糖的组成单糖有：Ｌ－鼠李糖、Ｌ－阿拉伯糖、Ｄ－半乳糖、Ｄ－甘露糖和Ｄ－半乳糠醛酸。     

高效液相色谱法测定淀粉中的顺丁烯二酸

建立了一种快速检测淀粉中顺丁烯二酸的高效液相色谱方法。确定的实验条件为:利用1 0%的乙醇提取样品,采用Shim-packVP-ODS柱(4.6 mm×1 50 mm,5μm),柱温3 0℃,检测波长2 20 nm,采用十六烷基三甲基溴化铵磷酸缓冲液与8 0%乙腈的混合物(体积比为8 0∶2 0)为流动相,流速1.0 mL/min。在确定的实验条件下,顺丁烯二酸在5～100 mg/L范围内线性关系良好,相关系数r=0.9999,平均回收率为9 8.56%,RSD=1.70%。本方法灵敏度高,结果准确、可靠,可以用于淀粉中顺丁烯二酸的含量检测。     

手性高效液相色谱法拆分儿茶酚胺类物质的进展

综述近年来高效液相色谱法拆分儿茶酚胺类物质的进展，对手性试剂衍生化法、手性流动相添加剂法和手性固定相法做了介绍。     

柱前衍生化-高效液相色谱法测定啤酒中的多胺

建立了用柱前衍生化高效液相色谱法分析啤酒中多胺的方法.在碱性介质中,多胺与1-(5-氟-2,4-二硝基苯基)-4-甲基哌嗪(PPZ)进行衍生化反应生成衍生物.实验采用Diamonsil C18(2)(迪马,150mm×4.6mm,3μm)色谱柱,以水-有机溶剂(乙腈-甲醇,体积比为6∶4)作为流动相,流速为0.5mL/min,用梯度洗脱程序方法同时分离5种多胺衍生物,衍生物的检测波长为362nm.通过考察方法的线性范围、稳定性、检测限和回收率表明:本方法具有样品处理简单、灵敏度高、速度快的优点,可用于啤酒中多胺含量的测定.     

二醇柱高效液相色谱法测定人参提取液中的人参皂苷

采用二醇柱,在等度洗脱条件下,建立了高效液相色谱(HPLC)定量分析人参提取液中人参皂苷的检测方法.优化的色谱条件:LiChrospher100 Diol柱(250 mm x2 mm i.d.,5μm),流动相为乙腈-水(体积比为82∶18),流速为1.0 L.min-1,检测波长为200 nm,柱温为15℃.研究结果表明:在较低温度下,采用二醇柱分析7种主要人参皂苷,具有分析速度快,不需要梯度洗脱程序,方法简单等优点.     

HPLC法分析洋葱中黄酮类化合物

通过盐酸水解,利用高效液相色谱法(HPLC)测定洋葱中槲皮素的含量,结合高效液相与质谱联用技术(HPLC-MS)鉴定洋葱水解样品中黄酮苷元.为测定洋葱中黄酮类化合物的含量,培育高含量黄酮类化合物的洋葱品种提供灵敏、准确和快速的测定方法.     

Enantiomeric separation of phenylsuccinic acid by cyclodextrin-modified reversed phase high-performance liquid chromatography

The chiral separation of phenylsuccinic acid (PSA) was studied by reversed phase high-performance liquid chromatography (RP-HPLC) with cyclodextrins (CDs) as chiral mobile phase additives. The effects of types of CDs, concentration of hydroxypropyl-β-cyclodextrin (HP-β-CD), percentage of organic modifier, pH value and column temperature on enantioselective separation were investigated. The quantification property of the developed RP-HPLC method was examined. The chiral recognition mechanism of PSA was also discussed. The results show that a baseline separation of PSA enantiomers is achieved on a Lichrospher C18 column (4.6 mm (inner diameter)×250 mm, 5 μm) with HP-β-CD as chiral mobile phase additive. The capacity factors of R-PSA and S-PSA are 3.94 and 4.80, respectively. The separation factor and resolution are respectively 1.22 and 8.03. The mobile phase is a mixture of acetonitrile and deionized water (20:80, volume ratio) containing 10 mmol/L HP-β-CD and 0.05% trifluoroacetic acid (pH 2.5, adjusted with triethylamine) with a flow rate of 1.0 mL/min. The ultraviolet (UV) detector is set at 254 nm. The likely roles are inclusion interaction, induction and hydrogen bonding between HP-β-CD and PSA enantiomers. Foundation item: Project(20776038) supported by the National Natural Science Foundation of China     

Preparative optimization of cellulose microspheres applied as supports for high-performance liquid chromatography

The aim of this work is optimizing the techniques to prepare pure cellulose microspheres, which are used as packing adsorbents for high-performance liquid chromatography. Thereupon, cellulose was dissolved in a pre-cooled NaOH/urea solution, from which various-size microspheres were prepared. The volume-average diameters were controlled approximately at 30 μm, 8 μm and 4 μm grades when cyclohexane, liquid paraffin and pump oil were used as dispersants, respectively. The present investigations reveal that higher viscosity dispersant is suitable for the preparation of smaller-size microspheres, while larger size microspheres are prepared preferably using lower-viscosity dispersant. The chiral stationary phase derived from 8 μm grade microspheres can separate the enantiomers of efavirenz.     

反相高效液相色谱法同时测定多种β 内酰胺类抗生素

建立了一种在同一个色谱体系下同时测定生物样品中头孢拉定、头孢氨苄、头孢克洛、氨苄青霉素、阿莫西林等5种临床最常用的β 内酰胺类抗生素的高效液相色谱方法.采用C8色谱柱（Dupout C8柱，300?mm×4.6?mm），以HAC NaAC 缓冲溶液(pH值为3.6) 甲醇 (75∶25 )为流动相，于254?nm处检测，分离并测定了上述5种抗生素.5种抗生素可在20?min内分离，最低检出限可分别达到0.18，0.21，0.12，0.35，0.25?μg/mL.将该法用于血清及尿样中药物含量的测定取得了满意结果.5种药物在血清中的回收率均大于94.6%，而在尿样中回收率均大于88.3%.实验证明该方法操作简便、快速灵敏、准确.     

Determination of residual monomers in polycarboxylate superplasticizer using high performance liquid chromatography

A procedure was developed for the determination of residual monomers in polycarboxylate superplasticizer (PCs) by reversed-phase high performance liquid chromatography (RP-HPLC).Four kinds of residual monomers were well separated and determined on a SinoChrom ODS-BP (C18) column with mobile phases composed of acetonitrile and phosphate buffer solution.The monomers were detected by UV detector at 205 nm and quantitatively analyzed with an external standard method.For those residual monomers,the linear response ranged from 4.0×10-6 mol·L-1 to 2.0×10-3 mol·L-1.The determination limit of acrylic acid,sodium methylallyl sulfonate and 2-Acrylamido-2-methylpropane sulfonic acid was 0.02×10-5 mol·L-1,while that of methoxy-polyethylene glycol monoacrylate was 0.1×10-5 mol·L-1.The relative standard deviation (RSD) of high concentration samples was less than 1%,while that of the low concentration samples was between 1%-4%.The standard (additional) recovery ratio was 97.4% -104.2%.     

虫灵灭中吡虫啉和巴沙的同时测定

以ClC-ODS(150mm×6.0mm,5μm)为色谱柱,V(甲醇)∶V(水)(φ=0.2%氨水溶液)=55∶45为流动相,其体积流量为0.8mL/min;用SPD-6AV紫外检测器检测波长为270nm,柱温为室温,灵敏度为0.16AUFS.实验表明,吡虫啉的线性方程为A=481586.1c-2381.26,r=0.9989,回收率为108%,RSD=2.56%;巴沙的线性方程为A=74333.36c-686.096,r=0.9975,回收率为106%,RSD=0.34%;吡虫啉的相对标准偏差RSD=0.187%,巴沙的相对标准偏差RSD=2.29%;并对流动相和检测波长进行了优化,确定了最佳的流动相和检测波长.     

固相萃取-高效液相色谱法测定玉米中伏马毒素B_1

研究了固相萃取 高效液相色谱法测定玉米中伏马毒素B1的方法。玉米样品经乙腈 0.1mol/ml磷酸二氢钠(1+1)提取,提取液通过固相萃取柱净化,净化液经柱前衍生,ShimadzuSTRODS色谱柱分离,荧光检测器检测,外标法定量。对添加不同含量水平的伏马毒素B1,5次重复实验的平均回收率为82.1%～87.8%,变异系数(CV)为4.7%～7.8%,检测低限为0.020mg/kg。