HPLC法测定不同产地鱼腥草中不同部位芦丁的含量

建立测定鱼腥草中芦丁含量的高效液相色谱分析方法。使用Eclipse XDB-C18色谱柱(4.6×150 mm,5μm),流动相为(A:0.1%磷酸水溶液,B:甲醇),柱温为20℃,流速为1.0 mL/min,检测波长为358 nm。测得芦丁的线性范围为0.02 mg/mL～0.50 mg/mL(r=0.9999),加标回收率为92.0%(n=3)。不同产地中芦丁含量测定结果表明,贵州产区的含量最高,河南的最低。不同部位中芦丁含量测定结果表明,叶中的含量均高于茎中5～10倍。本方法操作快速、简便、灵敏度高、重现性好,可使用于中草药中芦丁含量的测定。     

HPLC测定板蓝根中靛玉红含量的方法

目的:建立板蓝根中靛玉红含量测定方法.方法:用HPLC法,色谱柱:Shim-packCLC-ODS(150 mm×6mm),流动相:甲醇:氯仿(80:20)(0.1%二乙氨,用醋酸调中性),流速:1 mL/min,检测波长:290 nm,柱温:24℃.结果:靛玉红在1.058～16.928 μg/mL的浓度范围内具有良好的线性关系(r=0.999 98),精密度RSD=1.02%,加样回收率为96.87%,重现性RSD=0.94%.结论:本法简单可行,准确性好,重现性高,是板蓝根中靛玉红含量测定的有效方法.     

RP-HPLC法测定不同产地蓬子菜中二个黄酮类成分的含量

目的:测定10个产地蓬子菜中喇叭茶苷和香叶木苷的含量,建立蓬子菜中黄酮类成分含量测定的方法;方法:HPLC法,色谱柱:Hypersil ODS2 5μm(200mm×4.6mm i.d);流动相:甲醇-水-冰醋酸(体积比30:70:0.20);检测波长:340nm.结果:香叶木苷在0.601 0～1.510 μg(r=0.999 9),喇叭茶苷在0.098～0.249 8μg(r=0.996 2)与峰面积线性关系良好.结论:这两个黄酮类成分在10个产地中含量比较稳定,本法简单可行,准确性好,重现性高,是蓬子莱中黄酮类成分含量测定的有效方法.     

RP-HPLC法测定垫状卷柏中穗花杉双黄酮的含量

本文用反相高效液相色谱法测定垫状卷柏药材中的穗花杉双黄酮.选用Puraspher star RP-C18色谱柱(250 mm×4.6 mm,5μm),以甲醇-0.1%磷酸水溶液(65:35)为流动相,流速为0.8 mL/min,检测波长337 nm,柱温25℃进行检测.结果显示,穗花杉双黄酮的含量在0.038～0.342 μg范围内时进样量与峰面积积分值呈良好的线性关系,r=0.9999,平均回收率为101.2%,RSD为2.3%(n=6).该方法测定垫状卷柏药材中的穗花杉双黄酮含量灵敏、准确、重现性好.     

反相高效液相色谱法同时测定车前子中的毛蕊花苷和异毛蕊花苷

采用反相高效液相色谱法在Waters Symmitry C18(5 μm,250 mmm×4.6 mm)色谱柱上以甲醇:体积分数0.1%甲酸溶液(40:60,v:v)为流动相同时测定车前子中毛蕊花苷和异毛蕊花苷的含量,流动相流速为0.6 mL/min,检测波长为330 nm.毛蕊花苷线性范围为0.2～2.0 μ,r=0.9982.异毛蕊花苷线性范围为0.2～2.0 μ,r=0.9957.样品的平均回收率分别为99.70%,101.18%.测得大粒车前子中毛蕊花苷含量为8.65 mg/g,异毛蕊花苷含量为1.36 mg/g.此方法准确、快速,适用于车前子中毛蕊花苷和异毛蕊花苷的定量分析.     

不同产地滇重楼须根中氨基酸类成分的UPLC分析与评价

建立柱前衍生-超高效液相色谱法测定滇重楼须根中15种氨基酸含量,对不同产地样品进行分析评价。采用UPLC-PDA仪器,使用ACQUITY UPLC BEH C_(18)色谱柱(2.1 mm×150 mm,1.7μm),流动相A为0.1 mol/L乙酸钠溶液(冰醋酸调节pH=6.5)-乙腈(97∶3),B为乙腈-水(4∶1),梯度洗脱,检测波长254 nm,流速0.2 mL/min。滇重楼须根中检出15种氨基酸线性关系良好(r≥0.999 7),平均回收率RSD均小于3.00%。各产地均以天门冬氨酸和谷氨酸含量为最高,栽培滇重楼须根氨基酸平均含量高于野生品。本研究建立了分析评价滇重楼须根中氨基酸类成分的方法,为滇重楼须根的资源开发与利用提供科学依据。     

反相高效液相色谱法测定柳枝皮提取物中水杨苷的含量

建立了一种反相高效液相色谱法测定柳枝皮提取物中水杨苷的含量.色谱柱为Shim-pack CLC-ODS(6.0 mm i.d×150 mm,5 μm),流动相为甲醇-0.01 mol/L磷酸二氢钾水溶液(体积比为20∶80),在213 nm波长处检测.研究结果表明:水杨苷的检测限为25 ng,线性范围为8.00～80.00 mg/L,回归方程为A=0.0642C(241.2501(r=0.999 5),加样平均回收率为94.32%.方法操作简便、快速、准确.     

不同地区红景天植物红景天苷含量比较研究

采用高效液相色谱法(HPLC)测定了6种不同地区红景天植物红景天苷含量.以甲醇为提取溶剂,室温超声提取45 min,HPLC测定条件:岛津C18柱(4.6×250 mm,5 μm);流动相为甲醇∶水=3∶7;柱温25℃;检测波长为275 nm.结果表明,红景天苷含量分别为:大花红景天0.36%,狭叶红景天(狮子七)0.32%,宽果红景天0.14%,白三七0.04%,在小丛红景天、洮河红景天中未检测到红景天苷.     

高效液相色谱法测定肌肽滴眼液中L-肌肽的含量及有关物质

目的:建立肌肤滴眼液中L-肌肤的含量测定的HPLC方法.方法:采用Kromasil NH2色谱柱(200 mm × 4.6mm,5 μm),流动相为乙腈-40 mmol·L-1磷酸氢二钾溶液(44:56,磷酸调pH 6.3).流速1.0 mL·min-1,检测波长为210 ml,柱温为35℃.结果:肌肤在9.93～99.3μg·mL-1范围内线性关系良好(r=0.999 8),平均回收率为99.8%(RSD=1.0%,n=9),滴眼液中含L-肌肽的标示百分含量为97.0%～102.0%.结论:该方法操作简便、重复性好、专属性强,可用作肌肤滴眼液中L-肌肽的质量控制.     

不同产地玛咖中酰胺含量分析

建立玛咖酰胺测定方法,测定不同产地玛咖切片中玛咖酰胺含量。采用HPLC法,色谱条件为Sepax Sapphire C18色谱柱(250 mm×4.6 mm,5μm)流动相:乙腈(A)-0.05%磷酸水溶液(B),梯度洗脱:0~15 min,90%~95%A;15~50 min,95%A。检测波长208 nm,体积流量1.0 m L/min,柱温30℃。酰胺1、酰胺2、酰胺3分别在0.88~132μg/m L、0.85~128μg/m L、0.96~144μg/m L线性关系良好。酰胺1、酰胺2平均回收率分别为99.21%(RSD=1.64%)、98.59%(RSD=1.75%)。不同产地玛咖中玛咖酰胺含量差别较大,建立可靠、准确、重复性好的检测方法,有利于评价不同产地玛咖的质量。     

Investigation of the mechanism of temperature sensitivity of the electroreceptors of ampullae of lorenzini

In experiments on Black Sea skates (Raja clavata), the potential of the receptor epithelium of the ampullae of Lorenzini and spike activity of single nerve fibers connected to them were investigated during electrical and temperature stimulation. Usually the potential within the canal was between 0 and –2 mV, and the input resistance of the ampulla 250–400 k. Heating of the region of the receptor epithelium was accompanied by a negative wave of potential, an increase in input resistance, and inhibition of spike activity. With worsening of the animal's condition the transepithelial potential became positive (up to +10 mV) but the input resistance of the ampulla during stimulation with a positive current was nonlinear in some cases: a regenerative spike of positive polarity appeared in the channel. During heating, the spike response was sometimes reversed in sign. It is suggested that fluctuations of the transepithelial potential and spike responses to temperature stimulation reflect changes in the potential difference on the basal membrane of the receptor cells, which is described by a relationship of the Nernst's or Goldman's equation type.I. P. Pavlov Institute of Physiology, Academy of Sciences of the USSR, Leningrad. I. M. Sechenov, Institute of Evolutionary Physiology and Biochemistry, Academy of Sciences of the USSR, Leningrad. Pacific Institute of Oceanology, Far Eastern Scientific Center, Academy of Sciences of the USSR, Vladivostok. Translated from Neirofiziologiya, Vol. 12, No. 1, pp. 67–74, January–February, 1980.     

Determination of stoichiometry of radioiodination of proteins

A sensitive method for the detection of small quantities of hydrophobic antioxidant free radical scavengers such as butylatedhydroxytoluene (BHT) and butylatedhydroxyanisole (BHA) in aqueous samples is described. The procedure involves extraction of the hydrophobic free radical scavenger into an organic solvent phase, followed by the subsequent reaction of an aliquot of this extract with the stable cation radical tris(p-bromophenyl)amminium hexachloroantimonate (TBACA). In experiments with BHT and BHA, the loss of TBACA absorbance at 730 nm was found to be linearly proportional to the amount of antioxidant added, with quantities of BHT as small as 200 pmol being easily detectable. In aqueous suspensions of dimyristoylphosphatidylcholine vesicles, assays of the aqueous BHT concentration showed that BHT partitioned strongly into the membrane phase, achieving very high BHT/phospholipid ratios. For a given concentration of BHT, partitioning into the membrane phase was greater in large, multilamellar liposomes than in either small, single-walled vesicles or in purified rat brain synaptic vesicle membranes. Direct assay of BHT and BHA in phospholipid membranes, however, was complicated by a nonspecific interaction between TBACA and the phospholipid.