不同产地不同部位巫山淫羊藿中黄酮的HPLC分析

建立HPLC梯度洗脱法同时测定巫山淫羊藿中3种黄酮:淫羊藿次苷Ⅰ,朝藿定C和淫羊藿苷质量分数的方法。采用HPLC法,色谱柱为phenomenex C18分析柱(5μm,4.6 mm×250 mm);流动相为(A)水,(B)乙腈;柱温35℃;流速1.0 mL/min;检测波长270 nm;线性梯度洗脱条件:B∶15%(5 min),B∶30%(10 min),B∶50%(30 min)。本方法测定淫羊藿次苷Ⅰ,朝藿定C和淫羊藿苷的线形范围在0.20—1.80μg,r=0.999 3,r=0.999 9和r=0.999 7;平均回收率分别为98.43%,97.58%和97.91%,RSD(n=3)分别为2.16%,1.77%和1.90%。该方法简便、准确、重现性好,可作为同时测定淫羊藿次苷Ⅰ,朝藿定C和淫羊藿苷质量分数的方法。     

不同品种淫羊藿的淫羊藿苷含量研究

目的:比较不同品种淫羊藿的淫羊藿苷含量差异。方法:以十八烷基硅烷键合硅胶为填充剂,乙腈-水(30∶70)为流动相,检测波长270 nm,流速1.0 mL/min。结果:柔毛淫羊藿、朝鲜淫羊藿、淫羊藿(产自2个不同地方)的淫羊藿苷含量分别为0.28%、0.14%、0.83%和0.87%。结论:不同品种的淫羊藿所含淫羊藿苷的含量存在较大差异。品种的不同会影响淫羊藿药材的质量。     

不同酶对巫山淫羊藿中淫羊藿苷和朝藿定C含量的影响及抑菌活性研究

在巫山淫羊藿提取物中分别加入α-淀粉酶、果胶酶、纤维素酶进行酶解,经大孔树脂纯化后采用HPLC法测定巫山淫羊藿中淫羊藿苷和朝藿定C含量;并初步研究了巫山淫羊藿提取物对金黄色葡萄球菌和大肠杆菌的抑菌活性.结果表明,巫山淫羊藿提取物在经过酶解和纯化后,淫羊藿苷和朝藿定C的含量均明显增加,其中果胶酶对两者含量的影响最大,巫山淫羊藿提取物在经过果胶酶酶解和大孔树脂纯化后,淫羊藿苷和朝藿定C的含量分别增至11.65％、31.79％;巫山淫羊藿提取物及果胶酶酶解物对金黄色葡萄球菌和大肠杆菌均有较好的抑菌效果,但未酶解的巫山淫羊藿提取物的抑菌活性优于酶解物和纯化物.     

HPLC法测定不同产地淫羊藿药材中朝藿苷丙的含量

目的:建立高效液相色谱测定朝藿苷丙含量的方法。方法:采用Agilent Zorbax SB-C18柱,流动相为乙腈和水,检测波长270nm。结果:朝藿苷丙进样量0.02~2.00范围内线性良好,r=0.9996(n=6),加样回收率98.49,RSD=1.11%;10批淫羊藿药材中朝藿苷丙的含量为0.02%~0.88%。结论:朝藿苷丙为淫羊藿药材中的特征成分,其提取及含量测定方法操作简便,结果可靠,可作为淫羊藿药材质量控制的指标性成分。     

HPLC法测定更年三号胶囊中淫羊藿苷的含量

用HPLC法建立了测定更年三号胶囊中淫羊藿苷的含量的方法:采用高效液相色谱法,色谱柱为C18柱(250 mm×4.6 mm,5μm),乙腈-水(30∶70)为流动相,流速1.0 mL/min,检测波长为268 nm;进样量为10μL,室温进行检测。结果表明淫羊藿苷在0.2～8μg范围内进样量与峰面积呈良好的线性关系(r=0.9999),供试品溶液在24 h内稳定,平均回收率为100.49%(RSD=1.49%)。该方法简单快速,精密度高,稳定性较好,结果准确可靠,可以用于更年三号胶囊中淫羊藿苷的含量测定。     

超声波法提取淫羊藿中淫羊藿苷工艺研究

对超声波辅助提取淫羊藿中淫羊藿苷进行研究,以淫羊藿苷为考察目标,系统考察了超声波频率、乙醇浓度、超声提取时间、料液比四个因素对提取效果的影响。通过正交实验初步确定最佳提取工艺条件为:90%乙醇,超声波功率900 W,提取时间60 min,料液比1∶20。     

HPLC法测定太和春胶囊中淫羊藿苷的含量

建立了HPLC法测定太和春胶囊中淫羊藿苷含量的方法。采用KromasilC1 8(1 50mm× 4 .6mm ,5μm)色谱柱 ,以乙腈 水 (30∶70 )为流动相 ,流速 1 .0ml/min ,检测波长 2 70nm。结果表明 ,该法线性范围为3 .656mg/L～1 8.2 80mg/L,且相关系数良好 (r=0 .9999) ,平均回收率为 99.3 % ,RSD =1 .6 % (n =6)。本法快速、准确、简便 ,适用于太和春胶囊中淫羊藿苷的含量测定。     

淫羊藿苷提取工艺优化

通过正交实验优选淫羊藿苷的提取工艺,确定优化提取工艺条件为:60%乙醇、液固比为10∶1、提取1次、提取时间1.5 h,在此条件下淫羊藿苷的提取率为91.98%.     

粗毛淫羊藿抗炎活性成分研究

目的:研究粗毛淫羊藿的抗炎活性组分。方法:用100 ng·mL~(-1) LPS诱导RAW264.7细胞建立炎症筛选模型,测定促炎细胞因子IL-1β、IL-6、iNOS的m RNA表达变化确定炎症的程度;采用多种色谱方法对粗毛淫羊藿抗炎活性部位进行分离纯化;采用~1H-NMR,13C-NMR,ESI-MS等方法,结合文献数据,鉴定化合物结构。结果:粗毛淫羊藿甲醇提取物经大孔吸附树脂吸附,80%甲醇洗脱得到总黄酮部位,抗炎活性筛选具有抗炎活性,从中分离得到6个黄酮类化合物(1-6),结构分别鉴定为大花淫羊藿苷B(1),4"-鼠李糖基淫羊藿次苷Ⅱ(2),淫羊藿次苷Ⅱ(3),脱水淫羊藿素(4),淫羊藿苷(5),4"-鼠李糖基淫羊藿次苷Ⅱ(6),其中化合物2,3,4为首次从粗毛淫羊藿中分离得到。这些化合物都具有一定的抗炎活性。结论:总黄酮和化合物(1-6)对LPS诱导升高的促炎因子表达均具有下调作用,说明黔产粗毛淫羊藿总黄酮具有一定的抗炎活性,其活性成分为其中的黄酮和黄酮苷。     

淫羊藿总黄酮提取物树脂纯化工艺条件的优化

以D1400大孔树脂、HZ-841大孔树脂、PA03060聚酰胺树脂,通过动态吸附与洗脱,对淫羊藿总黄酮提取物进行纯化,HZ-841大孔树脂的纯化效果最优。通过正交试验得到最佳纯化工艺条件为:2g HZ-841大孔树脂,上样总黄酮含量2mg/mL的提取液30mL,分别以80mL水、40mL 20%乙醇、40mL85%乙醇和20mL 95%乙醇进行梯度洗脱,流速1.5mL/min。最优条件下,利用HZ-841树脂纯化淫羊藿总黄酮提取液,得到干浸膏收率3.25%,其中总黄酮含量71.8%,淫羊藿苷含量9.44%。     

Antioxidant activity of pilot‐plant alcoholic and supercritical carbon dioxide extracts of thyme

Leaves and flowering tops of thyme (Thymus vulgaris L.) were extracted with ethyl alcohol and supercritical carbon dioxide. Antioxidant activity was measured in sunflower oil at 0.3, 0.6 and 1% concentrations of extracts by oven test and Rancimat method. The activities of extracts were compared to those of butylated hydroxytoluene at 0.01 and 0.1% level. The ethanolic extract showed a slightly higher antioxidative effect than that obtained by supercritical fluid extraction. The effectiveness of both extracts added at 0.6% level were equal to that of 0.1% of butylated hydroxytoluene.     

Combination of supercritical fluid elution and resin adsorption for removal of procymidone from ginseng extracts

We propose a new method of resin adsorption (RA) coupled with supercritical fluid elution (SFE) for removal of pesticide residue and recovery of ginsenosides from ginseng extracts. D-101-1 resin was selected as the proper adsorption resin, acetone-n-hexane (4 : 6, v : v) served as the modifier with the flow rate of 1.5 mL/min during supercritical CO₂ elution of procymidone at 25 MPa, 55°C for 2 h, and absolute ethanol as the modifier at a flow rate of 1 mL/min for supercritical CO₂ elution of ginsenosides at 20 MPa, 60°C and 1 h. The results showed that the content of procymidone in the final products was only 0.0089 mg/kg. Meanwhile, the recovery rate of ginsenosides reached up to 92.5%. RA-SFE procedure provides an efficient approach to remove pesticide residue traces with little loss of active ingredients. The used resin can be recycled without any additional regeneration.     

Separation and purification of sulforaphane from broccoli by solid phase extraction

A simple solid-phase extraction (SPE) method for the determination of sulforaphane in broccoli has been developed. The optimal conditions were found to be use of a silica SPE cartridge, and ethyl acetate and dichloromethane as washing and eluting solvents, respectively, which could eliminate interferences originating from the broccoli matrix. The extracts were sufficiently clean to be directly injected into high-performance liquid chromatography (HPLC) for further chromatographic analysis. Good linearity was obtained from 0.05 to 200 μg/mL (r = 0.998) for sulforaphane with the relative standard deviations less than 3.6%. The mean recoveries of sulforaphane from broccoli were more than 90.8% and the detection limit (S/N = 3:1) was 0.02 μg/mL. The SPE method provides a higher yield of sulforaphane from crude extracts compared to conventional liquid-liquid extraction.     

反相液相色谱法测定7-羟基-3,4-二氢-2(1H)-喹啉酮的含量

建立了反相液相色谱测定7-羟基-3,4-二氢-2(1H)-喹啉酮含量的方法。采用shim-pack C18柱(5μm,4.6mmi.d.×250mm),流动相为v(甲醇)∶v[缓冲溶液(含事先配制好的0.075mol/L的磷酸二氢铵,磷酸调至pH=3)]=50∶50,流速为0.8mL/min,检测波长为250nm。外标法定量,7-羟基-3,4-二氢-2(1H)-喹啉酮1～100μg/mL浓度范围内呈良好的线性关系,线性回归系数r为0.9997,平均回收率为99.26%,RSD=1.17%(n=9)。     

Isolation and separation of tocopherols from olive by-products with supercritical fluids

Supercritical fluid extraction of olive pomace, the semisolid residue obtained using two-phase olive oil production systems, and supercritical fluid chromatographic separation of the extracts were performed to study the content of tocopherols, a group of compounds of interest for the food industry owing to their antioxidant activity. The developed method consists of supercritical CO₂ extraction at pilot plant scale and subsequent fractionation by two successive depressurizations. Enrichment of α-, β-, and γ-tocopherol was achieved in separator 2 when working at low densities in the first separator. Fractions obtained using high densities in separator 1 contained major proportions of triglycerides, waxes, and sterols. Tocopherols from olive by-products were separated and quantified in an environmentally friendly way by using supercritical fluid chromatography with packed capillary columns coated with polyethylene glycol and neat CO₂ according to a method previously optimized in our laboratory. The studied olive by-products can be considered a natural source of antioxidants because substantial concentration of tocopherols have been obtained in the extracts. The isolation and separation of tocopherols from olive pomace by applying supercritical fluid technology provides an interesting approach to exploit such by-products in an environmentally friendly way.     

高效液相色谱法测定小儿氨酚烷胺颗粒中对乙酰氨基酚的含量

建立了高效液相色谱法测定小儿氨酚烷胺颗粒中对乙酰氨基酚的方法。采用Eclipse XDB-C18色谱柱(4.6mm×150 mm,5μm),以甲醇—水(40：60)为流动相,流速为1.0 mL·min-1,检测波长为275 nm,进样量为20μL。结果表明,对乙酰氨基酚浓度在5.84～58.4μg·mL-1范围内与峰面...     

Fractionation of thyme (Thymus vulgaris L.) by supercritical fluid extraction and chromatography

Supercritical fluid chromatography (SFC) was employed to fractionate thyme (Thymus vulgaris L.) extracts, which were obtained by supercritical carbon dioxide extraction of thyme leaves. First, different supercritical extracts were produced at 313 K and at different pressures (15, 30 and 40 MPa). Thymol, a monocyclic terpenoid with recognized antiseptic, analgesic and anti-inflammatory properties, was identified and quantified in the different samples by GC-MS. Then, the supercritical extracts were fractionated by semi-preparative SFC, and different conditions such as pressure, temperature and amount of cosolvent (ethanol) employed were studied. Around a two fold increase of thymol was achieved at 15 MPa, 50 °C and 3% ethanol cosolvent, recovering 97% of the monocyclic terpenoid extracted.     

反相高效液相色谱法测定川楝子中阿魏酸含量

建立测定川楝子中阿魏酸含量的高效液相色谱法。采用VP-ODS C18（250 mm×4.6 mm,5μm）色谱分析柱;流动相为甲醇-1%冰醋酸（25：75）;检测波长：320 nm;流速：0.8 mL/min。结果阿魏酸进样量在0.25~2.50μg范围内与峰面积呈良好的线性关系（r=0.999 6）,平均加样回收率为99.38%,RSD=1.18%（n=6）。该方法简便、准确、可靠,可作为川楝子中阿魏酸的定量分析方法。