紫外导数分光光度法测定天麻中的天麻素和天麻甙元

样品用甲醇冷浸法提取。选用甲醇-乙醚(1 1)作为混合溶剂,采用二阶导数光谱可分离出天麻素和天麻甙元的吸收峰,在310～270nm间扫描,即可同时测定天麻中的天麻素和天麻甙元。方法简便,结果准确。样品中的其它组分不干扰测定。     

HPLC-DAD分析金线莲中天麻素和天麻苷元

研究超声-微波协同法提取金线莲中的天麻素和天麻苷元,并对提取条件进行了优化.应用高效液相-二极管阵列检测法分析提取物中的天麻素和天麻苷元.研究结果表明:金线莲中天麻素、天麻苷元和其他杂质成分能够很好的分离,且两者的含量分别为1.430及0.562 mg/g,相对标准偏差为0.94%和0.25%.方法准确、快速、灵敏度高、重现性好.     

共价有机框架材料TpBD-（NH2）2-D-（-）-α-苯甘氨酸用作高效液相色谱手性固定相的研究

该文采用溶剂热法合成了一种共价有机框架材料（COFs）TpBD-（NO2）2,将TpBD-（NO2）2还原为TpBD-（NH2）2后用D-（－）-α-苯甘氨酸对其进行手性修饰得到手性COFs材料TpBD-（NH2）2-D-（－）-α-苯甘氨酸。对TpBD-（NO2）2、TpBD-（NH2）2及TpBD-（NH2）2-D-（－）-α-苯甘氨酸3种COFs材料进行表征,并采用“网包法”制备了TpBD-（NH2）2-D-（－）-α-苯甘氨酸手性固定相。为考察该固定相的分离性能,将其用于制备高效液相色谱（HPLC）手性柱,并使用正己烷－异丙醇（体积比9∶1）和甲醇－水（体积比9∶1）为流动相,实现了13种手性化合物和5种苯系位置异构体的分离。且该色谱柱具有较好的重现性。实验表明TpBD-（NH2）2-D-（－）-α-苯甘氨酸用作HPLC固定相用于手性物质和苯系位置异构体分离具有良好的研究意义。     

毛细管电泳法测定天麻注射液中天麻素含量

报道了一种快速，准确的天麻注射液中天麻素含量的毛细管电泳测定法。方法的线性范围为８０－１５００μｇ／ｍＬ，ＲＳＤ＝１．９０％（ｎ＝６）加入回收率为９８．９－１０６．８％。     

苯溴马隆及其杂质的质量研究

建立了用HPLC和TLC两种方法测定新药苯溴马隆的杂质限量，以确保药物的质量，用反相HPLC法，ODS柱，甲醇－水－冰醋酸（88：12：2．5）（PH3．5）为流动相，检测波长254nm，流速1．0mL/min，分离出两种主要杂质，其结构已确证，在国内外文献中均未见报道。在制定苯溴马隆质量标准中，已将所建立RPHPLC法，作为该药物质的测定方法。     

色谱-串联质谱法测定天麻中53种禁用农药残留

建立超高效液相色谱-串联质谱联用（UPLC-MS/MS）及气相色谱-串联质谱联用（GC-MS/MS）法测定天麻中53种禁用农药残留。采用乙腈直接提取和基于QuEChERS原则的固相萃取法对样品进行处理。UPLC-MS/MS法采用电喷雾离子源，正离子模式下多反应监测，色谱峰面积外标法定量；GC-MS/MS法采用电子轰击离子源，色谱峰面积内标法定量。53种农药的质量浓度在一定范围内与响应值线性关系良好，相关系数均大于0.990，检出限为0.001～0.005 mg/kg，定量限为0.002～0.01 mg/kg。样品平均回收率为71.4%～118.2%，测定结果的相对标准偏差为1.4%～6.3%(n=6)。该方法能快速、有效地检测天麻中的禁用农药残留量，可用于天麻质量评价。     

三维荧光二阶校正法测定天麻中天麻素的含量

中药天麻背景复杂,对天麻素的激发-发射光谱(270nm/295nm)干扰特别大。本文利用三维荧光结合化学计量学二阶校正自加权交替三线性(SWATLD)算法对其进行解析,在不经分离的情况下测定了中药天麻中天麻素的含量。计算得到中药天麻中天麻素的平均含量是0.3766%,平均回收率为104.6%,分辨得到的天麻素解析光谱与真实光谱几乎完全重合。说明这种方法可用于中药天麻中天麻素含量的测定。     

天麻化学成分的研究

天麻的石油醚和70%乙醇提取部分经硅胶柱层析,分得八个成分(Ⅰ～Ⅷ)。Ⅶ[C₁₃H₁₈O₇,熔点145～148℃[α]_D¹⁵-66.4°,(C.0.65,水)]为天麻主要成分,根据光谱分析、衍生物制备和苦杏仁酶水解产物的鉴定,确定其结构为对羟甲基苯β-D-吡喃葡葡糖苷,命名为天麻苷。其余七个化合物分别鉴定为天麻苷元——对羟基苯甲醇(Ⅲ)、β-谷甾醇(Ⅱ)及其D-葡葡糖苷即胡萝卜苷(Ⅵ)、柠檬酸(Ⅴ)及其单甲酯(Ⅳ)以及棕榈酸(Ⅰ)和蔗糖(Ⅷ)。     

天麻的化学研究——Ⅰ.天麻化学成分的分离和鉴定

从中药天麻的乙醇提取物中分离得到7个化学成分。根据红外光谱、核磁共振谱、质谱分析,衍生物制备,以及已知样品对照,证明为天麻苷(天麻素)(Gastrodin)、对羟基苯甲醇、对羟基苯甲醛、琥珀酸、β谷甾醇、蔗糖及一微量而未确证的1,4-二取代芳环化合物。其中天麻素的化学结构为对羟甲基苯β-D-吡喃葡葡糖苷。     

制备型高效液相色谱法从积雪草提取物中分离纯化积雪草甙和羟基积雪草甙对照品

积雪草甙和羟基积雪草甙是积雪草及其相关制品质量控制的两个指标成分,本研究利用制备型高效液相色谱从积雪草提取物中同 时分离纯化得到这两个成分。对制备色谱的流动相组成、流速、进样量和检测波长等制备参数进行了优化。采用的色谱柱为C18柱(50 mm×200 mm,5 μm);流动相为甲醇-水(体积比为60∶40),流速100 mL/min;二极管阵列检测器在220 nm检测;进样体积为1.5 mL。在20 min的运行时间内,积雪草甙和羟基积雪草甙与干扰成分得到很好的分离,产品纯度达到98%以上。此方法具有快速高效、产品纯度高的 特点,可以用于制备积雪草甙和羟基积雪草甙对照品。     

Determination of gastrodin and vanillyl alcohol in Gastrodia elata Blume by pressurized liquid extraction at room temperature

Pressurized liquid extraction (PLE) at room temperature with a laboratory-assembled system was applied for the extraction of gastrodin (GA) and vanillyl alcohol (VA) in Gastrodia elata Blume. The proposed system setup for this current work was simpler as no heating and backpressure regulator was required. Extraction with PLE was carried out dynamically at a flow rate of 1.5 mL/min, at room temperature, under an applied pressure of 10-20 bars with an extraction time of 40-50 min. The extraction efficiencies of the proposed method using 20% aqueous ethanol were compared with heating under reflux using organic solvents such as methanol and ethanol/water (20:80) for different batches of medicinal plant materials. For the determination of GA and VA in G. elata Blume, the extraction efficiencies of PLE at room temperature were observed to be comparable with heating under reflux. The method precision was found to vary from 1.6 to 8.6% (RSD, n = 6) on different days. The marker compounds present in the various medicinal plant extracts were determined by gradient elution HPLC and HPLC/MS/MS. Our work demonstrated the possibility of implementation of PLE at room temperature and the advantages of minimizing the use of organic solvents in the extraction process.     

Preparative isolation and purification of gastrodin from the Chinese medicinal plant Gastrodia elata by high-speed counter-current chromatography

Gastrodia elata Blume is a famous Chinese medicinal plant, which has been widely used for the treatment of rheumatism, epilepsy, paralysis, hemiplegia, lumbago, headache and vertigo. High-speed counter-current chromatography was successfully used for the first time for the preparative isolation and purification of the bioactive component gastrodin from G. elata Blume. The crude gastrodin was obtained by extraction with ethanol from the dried roots of G. elata Blume under sonication. Preparative high-speed counter-current chromatography with a two-phase solvent system composed of n-butanol-ethyl acetate-water (2:3:5, v/v/v) was successfully performed yielding 48 mg gastrodin at 96% purity from 500 mg of the crude extract (10.3% gastrodin) with the recovery of approximately 90% in a one-step separation.     

Evaluation of the extraction efficiency of thermally labile bioactive compounds in Gastrodia elata Blume by pressurized hot water extraction and microwave-assisted extraction

Our earlier work showed that the stability of the bioactive compounds gastrodin (GA) and vanillyl alcohol (VA) in Gastrodia elata Blume behaved differently with varying compositions of water-ethanol using pressurized liquid extraction (PLE) at room temperature. To have a better understanding of the extraction process of these thermally labile compounds under elevated temperature conditions, pressurized hot water extraction (PHWE) and microwave-assisted extraction (MAE) methods were proposed. PHWE and MAE showed that GA and VA could be extracted using pure water under optimized conditions of temperature and extraction time. The extraction efficiency of GA and VA by the proposed methods was found to be higher or comparable to heating under reflux using water. The marker compounds present in the plant extracts were determined by RP-HPLC. The optimized conditions were found to be different for the two proposed methods on extraction of GA and VA. The method precision (RSD, n=6) was found to vary from 0.92% to 3.36% for the two proposed methods on different days. Hence, PHWE and MAE methods were shown to be feasible alternatives for the extraction of thermally labile marker compounds present in medicinal plants.     

高效液相色谱-蒸发光散射检测法测定蛋黄卵磷脂的含量

建立了蛋黄磷脂中卵磷脂（即磷脂酰胆碱,PC)的高效液相色谱-蒸发光散射检测（HPLC-ELSD）的测定方法。以Nov a-Pak Silica 60A硅胶柱(3.9 mm i.d.×150 mm,4 μm)为分离柱,正己烷-异丙醇-3%冰醋酸水溶液(体积比为35∶65 ∶8)为流动相，等度洗脱,流速1.0 mL/min,柱温30 ℃。蒸发光散射检测器漂移管温度50 ℃,雾化气(空气)压力350 kPa。在上述条件下测得PC在0.16~1.61 g/L范围内线性关系良好(r2=0.9979),检测限为0.64 μg,方法的精密度为3.2%(n=5),回收率为98.2%~128.2%。将该方法用于实际样品的测定,获得了令人满意的结果。该方 法预处理简单,分析速度快,可用于蛋黄磷脂中卵磷脂的测定。     

高效液相色谱分离-蒸发光散射检测法测定海藻糖的纯度

用反相高效液相色谱法分离－蒸发光散射检测法测定了海藻糖的纯度,检测下限为5mg/L。在30－1000mg/范围内,海藻糖浓度的对数与ELSD测得的峰面积对数具有良好的线性关系。     

Simultaneous determination of p-hydroxybenzaldehyde, p-hydroxybenzyl alcohol, 4-(beta-D-glucopyranosyloxy)-benzyl alcohol, and sugars in Gastrodia elata blume measured as their acetylated derivatives by GC-MS

A method for the simultaneous separation and determination of the active constituents and three sugars in the roots of Gastrodia elata Blume (GE), which is used as a famous Chinese traditional herbal medicine, by gas chromatography-mass spectrometry is established. The samples are acetylated with pyridine-acetic anhydride. The contents of 4-hydroxybenzaldehyde, 4-hydroxybenzyl alcohol (HA), fructose, glucose, 4-(beta-D-glucopyranosyloxy)-benzyl alcohol (GA), and sucrose in GE are 0.004%, 0.03%, 1.36%, 1.12%, 1.97%, and 4.25%, respectively, and the detection limits are 1.5, 3.0, 11.0, 5.0, 33.0, and 35.0 pg, respectively. The contents of HA and GA in the urine and brain of a mouse are also determined. This method is simple, reliable, and quick for the simultaneous determination of the active constituents and sugars in GE.     

离子排斥柱分离 /蒸发光散射检测同时测定天冬氨酸钾镁-山梨醇注射液中的天冬氨酸和山梨醇

 采用TSKgelOApak A离子排斥柱分离、蒸发光散射检测同时测定了天冬氨酸钾镁 山梨醇注射液中的天冬氨酸和山梨醇。在流动相为水 (含 0 1% (体积分数 )三氟乙酸 ) 甲醇 (体积比为 9∶1)溶液、柱温为室温的条件下 ,天冬氨酸和山梨醇的质量浓度为 2 0 0mg/L～ 2 0 0 0mg/L时与其峰面积具有良好的线性关系 (r =0 999)。该方法对天冬氨酸和山梨醇的检测下限分别为 30mg/L和 2 0mg/L。测定结果表明 ,该注射液的光、热稳定性非常好。     

复方丹参片中四种成分的高效液相色谱-电化学检测-紫外检测法分析

建立了电化学检测器与二极管阵列检测器联用的液相色谱(HPLC-ECD-DAD)同时分离和测定复方丹参片中原儿茶酸、原儿茶醛、咖啡酸和丹参酮ⅡA 等4种成分的分析方法。采用Zorbax SB-C18柱(150 mm×4.6 mm i.d.,5.0 μm),以甲醇和0.4%磷酸为流动相(流速1.0 mL/min)进行梯度洗脱;ECD检测电压0.7 V,DAD检测波长270 nm,柱温30 ℃。实验结果表明,原儿茶酸、原儿茶醛、咖啡酸和丹参酮ⅡA质量浓度分别为0.3～9.0 mg/L,1.1～54.0 mg/L,1.1～11.1 mg/L和5.2～52.0 mg/L时与其峰面积呈良好的线性关系(线性相关系数均高于0.999),原儿茶酸、原儿茶醛、咖啡酸和丹参酮ⅡA的平均回收率(n=6)分别为97.8%(相对标准偏差(RSD)为2.15%),98.2%(RSD为2.07%),97.6%(RSD为2.18%)和97.2%(RSD为2.07%)。该法同时利用了ECD和DAD的优点,是一种快速、灵敏、准确的分析方法,可以为复方丹参片的质量控制提供科学依据。     

高效液相色谱-蒸发光散射检测法测定藜芦中的介藜芦碱和藜芦胺

建立了高效液相色谱-蒸发光散射检测(HPLC-ELSD)测定藜芦中介藜芦碱、藜芦胺含量的方法,并对4种藜芦属药材样品进行了测定。采用的色谱柱为Kromasil C18柱(250 mm×4.6 mm, 5 μm),以乙腈和0.1%三氟乙酸水溶液为流动相进行梯度洗脱,洗脱程序为:0～5 min, 20%乙腈; 5～30 min, 20%乙腈～40%乙腈, 30～40 min, 40%乙腈～20%乙腈; 40～45 min, 20%乙腈;流速为0.8 mL/min;柱温为35 ℃;采用ELSD检测,漂移管温度为98 ℃,载气流速2.2 L/min 。介藜芦碱和藜芦胺的线性范围分别为42.05～980 mg/L和43.77～1020 mg/L;平均回收率分别为99.2%和101.4%,相对标准偏差分别为1.7%和2.1% (n=6);信噪比为3时,测得介藜芦碱和藜芦胺最低检测限分别为18.37 mg/kg和21.50 mg/kg。该方法快速简便、灵敏度和分离度好,适用于藜芦药材中活性生物碱的测定。     

微流控芯片非接触电导法测定感冒药中盐酸伪麻黄碱和氢溴酸右美沙芬

研究了用微流控芯片非接触式电导法分离检测感冒药日夜百服咛片中的两种主要成分盐酸伪麻黄碱和氢溴酸右美沙芬的方法。优化条件为:缓冲液20 mmol/L Tris 20 mmol/L H3BO3(pH=8.0);进样电压300 V;进样时间10.0 s;分离电压3.0 kV。非接触电导检测器激发电压60 V(Vp-p),频率60 kHz。两种成分的线性范围分别为20~1000 mg/L和10~1000 mg/L;检出限分别为10和5.0 mg/L;样品回收率分别为99.3%和97.6%。