正交试验法优选都梁凝胶贴剂的提取工艺

采用超声法优选都梁凝胶贴剂中白芷、川芎药对的最佳提取工艺.按照L9（34）正交试验设计,以欧前胡素、阿魏酸的转移率及干浸膏得率为综合评价指标,用高效液相色谱法进行含量测定.结果表明,都梁凝胶贴剂中白芷、川芎药对的最佳超声提取工艺为：8倍量的80％乙醇提取2次,每次超声40min;此时浸膏中欧前胡素的平均含量为0.1379％,阿魏酸的平均含量为0.1410％.本实验所建立的高效液相色谱法的准确度、精密度与重现性良好;提取工艺简便,合理.     

前胡内酯肟酯衍生物的合成及其抑制乙酰胆碱酯酶活性评价

本文以香豆素类化合物前胡内酯为先导化合物,设计合成了12个前胡内酯肟酯衍生物,所有目标化合物经熔点、~1H NMR和MS进行结构确证。体外抑制乙酰胆碱酯酶(AChE)活性评价结果表明,在1μmol/mL浓度下,目标化合物4a和4k对AChE具有较强的抑制活性,其抑制率分别达到58.05%和66.27%。初步构效关系研究表明,引入吲哚环能提高前胡内酯对AChE的抑制活性。通过分子对接方法考察了化合物4k与AChE结合的模式,发现目标化合物可以和AChE的催化活性中心部位结合。     

Crystallographic analysis of 9-(3-methylbut2-enyloxyfurano)[3,2-g] benzopyran-2-one

This structure of 9-(3-methylbut-2-enyloxyfurano)[3,2-g] benzopyran-2-one has been determined by X-ray diffraction methods. The compound crystallizes in the triclinic (space group P \(bar 1\)) with the unit cell parameters a = 11.1150(10), b = 11.8240(10), c = 11.9290(10) Å, α = 64.90(1)^°, β = 83.53(1)^°, γ = 89.25(1)^° and Z = 4. The structure has been solved by direct methods and refined to reliability index of 0.043. The unit cell contains two crystallographically independent molecules in the asymmetric unit, which exhibit different side-chain conformations. The crystal structure is stabilized by the intra molecular and intermolecular C–H?sO interactions.     

Supercritical fluid extraction for identification and determination of volatile metabolites from Angelica dahurica by GC-MS

The volatile components of Angelica dahurica were obtained by supercritical fluid extraction (SFE) method. These oils obtained were analyzed by GC-MS (identification and determination of metabolites). The compounds were identified according to their retention indices and mass spectra (electron impact (EI), 70 eV). The effects of different parameters, such as pressure, temperature, flow rate of CO(2), and the amount of modifier, on the SFE of A. dahurica oil were investigated. A total of 50 compounds of SFE extracts were identified. Phellopterin (PO), isoimperatorin (IO), imperatorin (IM), alloimperatorin (AM), byakangelicin, isooxypeucedanin, and pimpinellin were the major coumarin compounds identified in A. dahurica SFE extracts. The quantitations of PO, IO, IM, and AM were then accomplished. The calibration curves showed good linearity (R(2) >0.99) in the concentration ranges tested. The recoveries were higher than 85%, with RSDs less than 10%. The GC-MS method was successfully validated and applied to the quantitation of A. dahurica.     

8-O-烯丙基-4,4'-二甲基花椒毒酚的合成及其抗增殖活性

以焦性没食子酸和乙酰乙酸乙酯为原料,经Pechmann反应、Williamson成醚、环化、还原和脱水等反应合成了新化合物8-O-烯丙基-4,4'-二甲基花椒毒酚(5),总收率32.0%,其结构经1H NMR,13C NMR和ESI-MS表征。抗增殖活性测试结果表明:5对人类肝癌细胞Hep G2、结肠癌细胞HCT和子宫癌细胞SA具有一定的抗增殖活性,其中对Hep G2的抑制活性最高,IC50为(27.57±1.00)μmol·L-1。     

液相色谱-串联质谱法测定白芷中3种香豆素

建立了白芷中欧前胡素,异欧前胡素和氧化前胡素的液相色谱-串联质谱分析法。白芷提取液经Waters XTerra-C18(150mm×3.9 mm,5μm)色谱柱分离,以1mmol/L乙酸铵溶液和乙腈为流动相进行洗脱,以电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,外标法定量。欧前胡素,异欧前胡素和氧化前胡素分别在0.05～10μg/mL,0.05～13μg/mL和0.1～120μg/mL范围内呈线性相关,相关系数(r)分别为0.9993,0.9991和0.9994,检出限分别为30,30和50 ng/mL,平均加标回收率为100.1%,99.4%和98.4%,相对标准偏差分别为2.2%,2.6%和2.8%(ρ=0.5μg/mL,n=6),该法可以满足同时检测白芷中欧前胡素,异欧前胡素和氧化前胡素的需求。     

RP-HPLC同时测定辛芷提取物中的木兰脂素和欧前胡素

建立了RP-HPLC同时测定辛芷提取物中木兰脂素和欧前胡素的含量。取辛芷鼻提取物,用甲醇溶解,0.45μm微孔滤膜过滤,取续滤液进样检测。采用Hedera C8分析柱(4.6mm×250mm,5μm),流动相为乙腈-水(50∶50,V/V),流速1mL/min,柱温25℃,检测波长为278nm。木兰脂素、欧前胡素的线性范围分别为21.88—350.00μg/mL(r=0.9996,n=5)、1.25—20.00μg/mL(r=0.9997,n=5),平均回收率分别为103.56%、102.79%。该法简便、快速,结果准确可靠。     

超高效液相串联质谱法同时测定中成药中5-甲氧基补骨脂素、8-甲氧基补骨脂素和欧前胡素

建立了同时测定中成药都梁滴丸中5-甲氧基补骨脂素、8-甲氧基补骨脂素和欧前胡素的超高效液相-串联质谱检测方法。都梁滴丸以甲醇超声提取45 min,提取液稀释后经Waters Oasis HLB固相萃取小柱净化,采用WatersACQUITY UPLC BEHC18(50 mm×2.1 mm,1.7μm)色谱柱,以乙腈(A)和水(B)为流动相进行梯度洗脱。采用电喷雾电离正离子模式,多反应监测模式检测,以保留时间和离子比定性,外标法定量。方法的定量限8-甲氧基补骨脂素和5-甲氧基补骨脂素均为0.3 mg/kg;欧前胡素为0.75 mg/kg。3种化合物在25~500μg/L范围内均呈线性,相关系数r0.99。在高,中,低三种添加水平的平均回收率为82.0%~107.4%日内精密度(RSD%)为1.1%~12%。     

Identification and quantification of the volatile constituents in Cnidium monnieri using supercritical fluid extraction followed by GC‐MS

The volatile components of Cnidium monnieri were obtained by supercritical fluid extraction (SFE) and analyzed by GC‐MS (identification and determination of metabolites). The compounds were identified according to their retention times and mass spectra. The effects of different parameters, such as extraction pressure, temperature, dynamic extraction time, flow rate of CO₂, on the SFE of C. monnieri extracts were investigated. A total of 14 compounds of SFE extracts were identified. Osthole (69.52%), bornyl acetate (10.03%), α‐pinene (4.71%), and imperatorin (2.42%) were the major compounds identified in C. monnieri SFE extracts. The quantitation of osthole and imperatorin were then accomplished. The linear calibration ranges were all 5–1000 μg/mL for osthole and imperatorin by GC‐MS analysis. The recovery of osthole and imperatorin were in the range 96.5–101.8%. The LODs for osthole and imperatorin were 1.0 and 0.6 μg/mL, respectively.     

Preparative isolation and purification of bergapten and imperatorin from the medicinal plant Cnidium monnieri using high-speed counter-current chromatography by stepwise increasing the flow-rate of the mobile phase

A high-speed counter-current chromatography (HSCCC) method was developed for the preparative separation and purification of bergapten and imperatorin from the Chinese medicinal plant Cnidium monnieri (L.) Cusson. The crude extract was obtained by extraction with ethanol from the dried fruits of Cnidium monnieri (L.) Cusson under sonication. Preparative HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-ethanol-water (5:5:5:5, v/v/v/v) was successfully performed by increasing the flow-rate of the mobile phase stepwise from 1.0 to 2.0 ml min(-1) after 180 min. The components purified and collected were analyzed by high-performance liquid chromatography. The method yielded 45.8 mg of bergapten at 96.5% purity and 118.3 mg of imperatorin at 98.2% purity from 500 mg of the crude extract in a single run. The recoveries of bergapten and imperatorin were 92.1 and 93.7%, respectively.