HPLC法测定嘎扎络舒凝胶剂中对甲氧基桂皮酸乙酯的含量

目的:建立HPLC法测定嘎扎络舒凝胶剂中对甲氧基桂皮酸乙酯的含量.方法:固定相为C18柱;流动相为甲醇-水(63:37);检测波长310nm.结果:对甲氧基桂皮酸乙酯的线性范围为0.08～0.48μg,r=0.99999.样品平均回收率为98.02%,RSD为1.89%.结论:本法简单,快速,结果准确,可作为该制剂的质量控制方法.     

Chemopreventive effects of wild carrot oil against 7,12-dimethyl benz(a)anthracene-induced squamous cell carcinoma in mice

Context: Daucus carota L. ssp. carota (Apiacea) is widely distributed throughout the world and has many uses in traditional medicine.

Objective: The present study investigates the chemopreventive effects of oil extract of D. carota umbels on 7,12-dimethyl benz(a)anthracene (DMBA)-induced skin cancer in mice.

Materials and methods: D. carota oil extract (DCOE) was prepared by extracting the dried umbels with 50:50 acetone:methanol. Skin papilloma were initiated by DMBA and promoted by 12-O-tetradecanoyl phorobol-13-acetate (TPA). The extract was administered to animals via gavage (0.02?mL of 100% oil), intraperitoneal (0.3?mL of 2% oil), and topical (0.2?mL of 5, 50, and 100% oil) routes for 20 weeks. Tumor appearance, incidence, yield, and volume were compared with those of a non-treated control group.

Results: Topical 100% treatment delayed tumor appearance, and inhibited tumor incidence and yield by 40 and 89%, respectively. Topical 50% treatment inhibited tumor incidence and yield by 30 and 83%, respectively, whereas the 5% treatment inhibited tumor yield by 36%. Tumor volume was decreased by 99, 91, and 70% following topical treatments with 100, 50, and 5% oil, respectively. Intraperitoneal treatment inhibited tumor yield by 43%, and decreased tumor volume by 85%, whereas gavage treatment showed minimal effects on both. Intraperitoneal and topical treatment decreased infiltration and hyperplasia with an increase in the level of hyperkeratosis.

Conclusion: These findings demonstrate that DCOE has remarkable antitumor activity against DMBA-induced skin cancer compared with non-treated animals paving the ground for further investigations.     

HPLC法测定不同品种川芎药材中阿魏酸的含量

目的用高效液相色谱法（HPLC）测定两种川芎药材中阿魏酸的含量,为选择川芎药材提供参考。方法建立了一种HPLC测定川芎药材中阿魏酸含量的方法。HPLC法采用Agilent TC-C18（4.6mm×150mm,5μm）色谱柱,以乙腈-0.085%磷酸溶液（17∶83）为流动相,流速1mL.min-1,检测波长316nm,柱温35℃。结果阿魏酸对照品溶液在0.01248~0.2496μg范围内线性关系良好,标准曲线方程为y=4853.4x-3.1533,r=0.9998,加样回收率的RSD是1.6%。结论采用此HPLC法测定两种川芎药材中阿魏酸含量,测定结果准确可靠。川芎中有效成分阿魏酸含量是东川芎的2倍多。     

决明子中蒽醌类成分在大鼠体内的药动学

目的:建立大鼠血浆中决明子蒽醌类成分的RP-HPLC定量分析方法,并用于大鼠体内蒽醌类药动学研究。方法:采用Zorbax Extend-C18(250 mm×4.6 mm,5μm)(Palo Alto,CA,USA)色谱柱,以乙腈-0.3%醋酸水为流动相进行梯度,流速1.0mL.min-1,检测波长258 nm,柱温28℃。采用RP-HPLC测定决明子中芦荟大黄素(aloe-emodin)、美决明子素(obtusifo-line)和大黄酚(chrysophanol)3个蒽醌类指标成分在大鼠血浆的浓度,并根据测定结果求算药动学参数。结果:建立了决明子中芦荟大黄素、美决明子素和大黄酚在大鼠血浆中的含量测定方法。实验结果表明蒽醌类成分在大鼠体内吸收迅速,消除也较快。结论:本方法简便、准确、专属性强,可以应用于大鼠灌胃给药决明子蒽醌类提取物后的药动学研究     

The anti-inflammatory activity of licorice,a widely used Chinese herb

Context: Increasing incidence and impact of inflammatory diseases have encouraged the search of new pharmacological strategies to face them. Licorice has been used to treat inflammatory diseases since ancient times in China.

Objective: To summarize the current knowledge on anti-inflammatory properties and mechanisms of compounds isolated from licorice, to introduce the traditional use, modern clinical trials and officially approved drugs, to evaluate the safety and to obtain new insights for further research of licorice.

Methods: PubMed, Web of Science, Science Direct and ResearchGate were information sources for the search terms ‘licorice’, ‘licorice metabolites’, ‘anti-inflammatory’, ‘triterpenoids’, ‘flavonoids’ and their combinations, mainly from year 2010 to 2016 without language restriction. Studies were selected from Science Citation Index journals, in vitro studies with Jadad score less than 2 points and in vivo and clinical studies with experimental flaws were excluded.

Results: Two hundred and ninety-five papers were searched and 93 papers were reviewed. Licorice extract, 3 triterpenes and 13 flavonoids exhibit evident anti-inflammatory properties mainly by decreasing TNF, MMPs, PGE2 and free radicals, which also explained its traditional applications in stimulating digestive system functions, eliminating phlegm, relieving coughing, nourishing qi and alleviating pain in TCM. Five hundred and fifty-four drugs containing licorice have been approved by CFDA. The side effect may due to the cortical hormone like action.

Conclusion: Licorice and its natural compounds have demonstrated anti-inflammatory activities. More pharmacokinetic studies using different models with different dosages should be carried out, and the maximum tolerated dose is also critical for clinical use of licorice extract and purified compounds.     

HPLC法同时测定活络消痛片中紫丁香苷、阿魏酸和丹酚酸B含量

目的:建立HPLC法同时测定活络消痛片中紫丁香苷、阿魏酸和丹酚酸B的含量。方法:色谱柱为Kromasil C18柱(150 mm×4.6 mm,5μm),流动相为甲醇-0.2%磷酸溶液,梯度洗脱,流速为1.0 ml·min-1,检测波长为紫丁香苷(265 nm),阿魏酸(321 nm),丹酚酸B(286 nm),柱温为25℃。结果:紫丁香苷、阿魏酸和丹酚酸B分别在64.500~1.032×103μg·ml-1、7.525~120.400μg·ml-1、65.250~1.044×103μg·ml-1范围内与峰面积呈良好的线性关系,平均回收率分别为100.75%、99.56%、99.75%。结论:本方法简便、准确、快速。     

HPLC法测定不同来源红花中对香豆酸的含量

目的:采用高效液相色谱法测定不同来源红花中对香豆酸含量。方法:采用Diamonsil C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.5%磷酸溶液(18∶82)为流动相,流速1.0 mL.min-1,检测波长308 nm,柱温30℃。结果:对香豆酸线性范围为0.0211~0.422μg.mL-1;平均回收率(n=6)为99.98%,RSD为1.2%。结论:该方法简便、准确,重复性好,可作为红花的质量控制方法。     

HPLC法同时测定杏花中阿魏酸、芦丁和异槲皮苷

目的建立HPLC法同时测定杏花中阿魏酸、芦丁和异槲皮苷。方法色谱柱为YMC-Pack ODS-A C_(18)柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.1%磷酸溶液(15∶85);体积流量1.0 mL/min;检测波长为343 nm;柱温为30℃。结果阿魏酸、芦丁和异槲皮苷分别在0.029 08~0.290 8μg(r=0.999 9)、0.548 4~5.484 2μg(r=0.999 9)、0.033 07~0.330 7μg(r=0.999 9)范围内线性关系良好;平均回收率分别为98.31%、98.93%、100.25%,RSD分别为1.0%、0.9%、1.1%。10批杏花样品中阿魏酸、芦丁、异槲皮苷含量测定结果分别为0.105~0.554、3.080~6.933、0.258~0.974 mg/g。结论该方法多种成分同时测定,操作简便、准确,重复性好,可用于杏花药材的质量控制。     

HPLC法同时测定抗敏颗粒中芍药苷、毛蕊异黄酮苷和阿魏酸的含量

目的:建立以高效液相色谱法同时测定抗敏颗粒中芍药苷、毛蕊异黄酮苷和阿魏酸含量的方法。方法:色谱柱为KromasiL C18(250mm×4.6mm,5μm),流动相为甲醇-乙腈-0.4%磷酸溶液(20∶10∶70),流速为1.0mL·min-1,检测波长为254nm,柱温为室温,进样量为10μL。结果:芍药苷、毛蕊异黄酮苷和阿魏酸的检测浓度分别在180～3600μg·mL-1(r=0.9992)、4.6～92.0μg·mL-1(r=0.9991)和8.0～160.0μg·mL-1(r=0.9994)范围内与各自峰面积积分值呈良好线性关系;平均回收率分别为98.3%(RSD=1.8%,n=9)、99.0%(RSD=2.0%,n=9)和100.5%(RSD=1.1%,n=9)。结论:本法操作简便、准确、灵敏、重现性好,可用于抗敏颗粒的质量控制。     

HPLC法对皂荚属植物中刺囊酸的含量测定

采用HPLC法 ,对皂荚属 3种植物果实中刺囊酸的含量进行了测定。用TSK ODS柱 ,流动相为甲醇 -水 (V∶V ,80∶2 0 ) ,在 2 15nm下检测。平均回收率为 95 1% ,RSD为 1 30 % ,所建立的方法确实可靠 ,具有良好的线性关系。本法可用于皂荚属植物的含量测定。刺囊酸在皂荚属植物中分布广泛 ,且含量较高 ,种间差异明显     

Dietary ferulic acid,biochanin A,and the inhibition of reproductive behavior in Japanese quail (Coturnix coturnix)

A study was conducted to determine the effects of two dietary compounds, biochanin A and ferulic acid, on the reproductive performance of Japanese quail, Coturnix coturnix. These compounds may be present in the diet of wild birds during dry years or at the end of the growing season during normal years. Four treatment groups, each fed a diet supplemented with biochanin A or ferulic acid, and a control group were tested for morphological and behavioral effects before, during and after treatment. Fertility and hatchability data were collected during treatment only. Ferulic acid was shown to inhibit male copulatory behavior during treatment. Biochanin A inhibited male copulatory behavior during and after treatment. Neither drug affected female copulatory behavior though egg-laying was inhibited by the low dose of biochanin A. Ferulic acid significantly reduced the hatchability of eggs. Biochanin A increased the fertility of males and the hatchability of eggs fertilized by them. A correlation between results of this study and natural conditions of reproduction is discussed. It is concluded that both biochanin A and ferulic acid exert inhibiting influences on the reproductive behavior of Coturnix.     

RP-HPLC测定贯叶连翘中金丝桃素、芦丁和槲皮素的含量

目的:采用高效液相法测定贯叶连翘中的金丝桃素、芦丁和槲皮素的含量方法.方法:色谱柱为Symmtry C18(4.6mm×250 mm,5μm),检测波长分别为588 nm,359 nm,流动相分别为甲醇-乙腈-1.0%磷酸二氢钠溶液(340:12:7)和甲醇-水(40:60).结果:线性范围分别在0.02704～0.1352μg和0.264～1.32μg,0.052～0.260μg内良好,回收率分别为98.39%(n=3)、98.56%(n=3)和98.85%(n=3).RSD分别为0.78%和1.01%和1.02%.结论:该法简便,精密度高,结果准确可靠.     

口服后莫达非尼及其代谢产物在汉族健康人体内的药物动力学

目的研究莫达非尼及其代谢产物(莫达非尼酸)在中国汉族健康人体内的药物动力学过程。方法10名健康志愿者口服莫达非尼片200 mg,采用HPLC法测定给药后不同时间点的莫达非尼及其代谢物的浓度,用DSA软件求算其药物动力学参数,并比较药物动力学参数在性别上的差异。结果莫达非尼及其代谢物莫达非尼酸的药物动力学过程符合二室模型拟合,其药物动力学参数分别为:莫达非尼tmax(1.69±0.70)h,ρmax(4.14±1.21)mg.L-1,AUC0-∞(65.96±11.69)mg.h.L-1;莫达非尼酸tmax(3.06±0.94)h,ρmax(3.19±0.95)mg.L-1,AUC0-∞(45.94±13.44)mg.h.L-1。结论口服莫达非尼在人体内其原形及代谢产物药物动力学均符合二室模型拟合,其药物动力学参数没有性别差异。     

单次口服莫达芬尼片在中国健康志愿者的药代动力学

目的研究单次口服莫达芬尼片的药代动力学。方法选择9名健康成年男性受试者分别单次口服100,200,300mg 3个剂量的莫达芬尼片后,用HPLC法测定血中原形药莫达芬尼及代谢产物莫达芬尼酸浓度,用3P97软件进行数据处理,计算药代动力学参数。结果原形药莫达芬尼的药-时曲线符合二房室模型,其主要药代动力学参数的Cmax、AUC0-∞、AUC0-t随剂量加大而增加;t1/2b、tmax、b、CL与给药剂量无关。莫达芬尼片原形药经肾排泄较少,48h经肾累积排泄率分别为(4.44±4.28)%,(3.35±2.20)%和(2.86±1.39)%。主要代谢产物莫达芬尼酸药-时曲线符合二房室模型,48h莫达芬尼酸经肾累积排泄率分别为(33.51±18.90)%,(32.36±19.92)%和(22.88±6.89)%。结论莫达芬尼在100～300mg内,呈线性动力学特征而无饱和性,其消除过程是经肝脏代谢,代谢产物为莫达芬尼酸,代谢产物主要经肾排泄。     

Simultaneous determination of danshensu, ferulic acid, cryptotanshinone and tanshinone IIA in rabbit plasma by HPLC and their pharmacokinetic application in danxiongfang

A selective and sensitive reversed-phase high performance liquid chromatography method was developed and validated for the simultaneous determination of danshensu, ferulic acid, cryptotanshinone, and tanshinone IIA in rabbit plasma using p-hydroxybenzoic acid as internal standard. Liquid–liquid extraction was used for sample preparation. Chromatographic separation was successfully achieved on an Agilent HC-C₁₈ column using a mobile phase composed of methanol–water (from 20:80 to 80:20, v/v) containing 0.5% (v/v) glacial acetic acid. The mobile phase was employing gradient elution at a flow rate of 1.0 ml/min. The method showed good linearity and no endogenous material interfered with the marked compounds and I.S. peaks. The limit of quantification of danshensu, ferulic acid, cryptotanshinone, and tanshinone IIA were 0.1, 0.03, 0.05, and 0.05 μg/ml, respectively. The average extract recoveries of the four compounds from rabbit plasma were all over 60%. The precisions determined from 5 days were all within 10%. The established method has been successfully applied in the pharmacokinetic study and drug interaction of danshensu, ferulic acid, cryptotanshinone, and tanshinone IIA in rabbits after intravenous administration of danxiongfang, a useful compound preparation of traditional Chinese medicine.     

新疆一枝蒿的质量标准研究

目的 对新疆一枝蒿药材的水分、总灰分、药材鉴别和酮酸含量测定等方面进行研究,建立新疆一枝蒿药材的质量标准.方法 采用<中华人民共和国药典>2005年版一部附录Ⅸ H 水分测定法中的烘干法和附录Ⅸ K 灰分测定法中总灰分测定方法检查药材的水分和总灰分;采用附录Ⅵ B薄层色谱法建立定性鉴别一枝蒿药材的方法;采用高效液相色谱法(附录Ⅵ D)测定新疆一枝蒿药材活性成分酮酸的含量.结果 新疆一枝蒿药材的含水量不得超过8.0%,总灰分不得超过16.0%;薄层色谱斑点清晰、专属性强;酮酸在5.60～56.00 μg范围内线性关系良好,回归方程Y=8.522 3X-6.150 7,r= 0.997 2,平均加样回收率为99.7%,RSD=0.25%.结论 该方法操作简便、准确快速、重复性好,有助于新疆一枝蒿药材的质量控制,可为药用植物资源的开发利用提供科学依据.     

HPLC法测定大鼠血浆中抗肿瘤化合物SYUIQ-5的浓度

目的建立一种灵敏度较高的高效液相色谱法,测定大鼠血浆中抗肿瘤化合物SYUIQ-5的浓度。方法流动相用35mmol·L-1磷酸氢二钾缓冲液(pH8.0)-甲醇-三乙胺(30∶70∶0.05),血浆样本用乙醚萃取,紫外检测波长为278nm。结果线性范围为30~1500μg·L-1,线性关系良好,最低检测限为20μg·L-1,日内RSD≤5.2%,日间RSD≤3.8%;提取回收率为72.1%~80.5%(n=5),相对回收率为96.8%~105.1%。结论本方法灵敏度高,重现性好,精密度和准确性好,适于SYUIQ-5的药代动力学研究。     

HPLC法同时测定通脉颗粒中丹参素、阿魏酸和葛根素的含量

目的:建立同时测定复方通脉颗粒中丹参素、阿魏酸和葛根素含量的方法。方法:采用高效液相色谱法测定。色谱柱为Agilent Zorbax SB-C18柱,流动相为乙腈-1%冰醋酸,流速为1.0mL·min-1。结果:丹参素、阿魏酸和葛根素的线性范围分别为2.95～29.5μg·mL-1(r=0.9999)、1.288～16.10μg·mL-1(r=0.9999)和5.26～52.6μg·mL-1(r=0.9997);平均加样回收率(n=6)分别为99.92%(RSD=1.53%)、100.0%(RSD=2.74%)和99.05%(RSD=1.46%)。结论:本方法简便、快速、可靠,可用于复方通脉颗粒的质量控制。