高效液相色谱法同时测定白带净丸中的3'-羟基葛根素、葛根素、尿囊素、川续断皂苷Ⅵ和茯苓酸的含量

目的建立同时测定白带净丸中3'-羟基葛根素、葛根素、尿囊素、川续断皂苷Ⅵ和茯苓酸的HPLC法。方法采用Dikma-C_(18)(250 mm×4.6 mm,5μm),以乙腈(A)-0.5%磷酸溶液(B)为流动相,梯度洗脱,流速0.9 mL·min~(-1),柱温30℃,进样量为10μL。结果 3'-羟基葛根素、葛根素、尿囊素、川续断皂苷Ⅵ和茯苓酸的线性范围分别为:6.14~122.80μg·mL~(-1)(r=0.9993),7.59~151.80μg·mL~(-1)(r=0.9991),4.15~83.00μg·mL~(-1)(r=0.9999),8.13~162.60μg·mL~(-1)(r=0.9994),5.35~107.00μg·mL~(-1)(r=0.9997);平均回收率及RSD均符合药典规定。结论所建方法重复性好,专属性强,可用于白带净丸的质量控制。     

高效液相色谱分离柱后化学发光法同时测定菟丝子中黄酮类成分

目的:建立高效液相色谱分离柱后化学发光法测定菟丝子中芦丁、山柰素、槲皮素和异鼠李素含量。方法:基于在氢氧化钠碱性介质中铁氰化钾可以直接氧化芦丁、山柰素、槲皮素和异鼠李素产生化学发光。色谱柱:Hypersil ODS(5μm,4.6 mm×150 mm),流动相:乙醇-乙腈-水-磷酸(21:22:55:2),流速:1mL·min~(-1),柱温:25℃。结果:芦丁、山柰素、槲皮素和异鼠李素浓度分别在0.2～5μg·mL~(-1)(r=0.9990),0.1～15μg·mL~(-1)(r=0.9991),0.1～100μg·mL~(-1)(r=0.9994),0.3～200μg·mL~(-1)(r=0.9998)范围内,与峰面积有良好的线性关系;检测限(S/N=3)分别为0.02,0.08,0.08,0.03μg·mL~(-1)。结论:水法简便、快速、有效,灵敏度高,首次用于菟丝子中黄酮类成分的测定,取得了很好的结果。     

HPLC法测定复方对乙酰氨基酚片中对乙酰氨基酚、乙酰水杨酸及咖啡因的含量

目的:采用高效液相色谱法测定复方对乙酰氨基酚片中对乙酰氨基酚、乙酰水杨酸及咖啡因的含量。方法:采用 Li-chrospher C_(18)(5 μm,4.6 mm×250 mm)色谱柱,以甲醇-水-冰醋酸(40:60:0.3)为流动相,流速1.0 mL·min~(-1),检测波长272 nm,柱温35℃。结果:对乙酰氨基酚线性范围为19.93～199.32μg·mL~(-1)(r=0.9998),平均回收率(n=9)为99.2%;乙酰水杨酸线性范围为36.00～359.96μg·mL~(-1)(r=0.9999),平均同收率(n=9)为99.7%;咖啡因线性范围为4.90～49.04μg·mL~(-1)(r=0.9998),平均同收率(n=9)为98.8%。结论:方法简使,结果准确,适用于该产品的质量控制。     

高效液相色谱法测定复方异维倍克气雾剂中异丙托溴铵和盐酸克仑特罗的含量

目的:建立高效液相色谱法测定复方异维倍克气雾剂中异丙托溴铵和盐酸克仑特罗含量。方法:采用反相高效液相色谱法。Intersil C_(18)分析色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-水(16:84;含0.4%三乙胺,磷酸调 pH 为3),流速1.5 mL·mL~(-1),检测波长205 nm。结果:异丙托溴铵和盐酸克仑特罗的理论板数分别为2400和3500。异丙托溴铵回归方程Y=128458X 58038,r=0.9999,线性范围18.20～182.0μg·mL~(-1);盐酸克仑特罗回归方程 Y=1251564X 10954,r=0.9995,线性范围9.200～46.00μg·mL~(-1)。异丙托溴铵平均回收率为97.4%(n=5),RSD 为2.2%;盐酸克仑特罗平均回收率为100.8%(n=5),RSD为1.9%。异丙托溴铵和盐酸克仑特罗最低检出浓度分别为0.2μg·mL~(-1)和0.03μg·mL~(-1)。结论:方法简便,结果准确。     

反相高效液相色谱法测定苯酰甲硝唑有关物质

目的:建立反相高效液相色谱法测定苯酰甲硝唑有关物质。方法:采用双波长检测,梯度洗脱。色谱柱为迪马公司 Dia-monsil~(TM)C_(18)(250mm×4.6mm,5μm);流动相 A 和 B 分别为1.5g·L~(-1)磷酸二氢钾溶液(用1mol·L~(-1)磷酸溶液调 pH3.2)-乙腈(80:20和58:42);流速1.0mL·min~(-1),检测波长为235,315nm,进样量20μL,柱温为室温,外标法和主成分自身对照法计算。结果:杂质 A、杂质 B、杂质 C、苯酰甲硝唑均能达到很好的分离,并分别在1.12～16.8μg·mL~(-1)(r=1.000),1.12～16.8μg·mL~(-1)(r=0.9999),1.0～15.0μg·mL~(-1)(r=1.000),1.04～15.6μg·mL~(-1)(r=0.9992)浓度范围内具有良好的线性关系。杂质 A、杂质 B、杂质 C 的平均回收率(n=9)分别为99.4%,99.6%,99.5%。结论:本法简便、灵敏、准确,专属性强,适合于苯酰甲硝唑有关物质的测定。     

HPLC法测定复方降压胶囊中氢氯噻嗪、地巴唑、氯氮(艹卓)和盐酸异丙嗪的含量

目的:建立离子对高效液相色谱法同时测定复方降压胶囊中氢氯噻嗪、地巴唑、氯氮(艹卓)和盐酸异丙嗪含量。方法:分析柱为 Hypersil C_(18)(4.6mm×250mm,5μm),流动相为乙腈-甲醇-7.2mmol·L~(-1)己烷磺酸钠溶液-冰醋酸-三乙胺(28∶28∶43∶1∶0.01),检测波长为258nm。结果:氢氯噻嗪、地巴唑、氯氮(艹卓)和盐酸异丙嗪的线性范围分别为12.24-122.4μg·mL~(-1)(r=0.9997),40.92-409.2μg·mL~(-1)(r=0.9998),8.12-81.2μg·mL~(-1)(r=0.9999),11.52-115.2μg·mL~(-1)(r=0.9999);平均回收率分别为100.3%(RSD<1.4%),99.0%(RSD<1.3%),98.8%(RSD<1.7%),99.4%(RSD<2.3%)。结论:4种组分分离效果好,其他组分和辅料无干扰,本法简便快速,准确可靠,适于该复方制剂中4种组分的同时测定。     

HPLC法同时测定乳块消片中丹参素、原儿茶醛、橙皮苷、丹酚酸B的含量

目的:采用 HPLC 法同时测定乳块消片中丹参素、原儿茶醛、橙皮苷、丹酚酸 B 4种成分的含量。方法:采用 Eclipse XDB-C_(18)色谱柱(4.6 mm×250 mm,5μm);以甲醇-3%醋酸水溶液为流动相梯度洗脱;流速为1 mL·min~(-1);柱温为30℃;检洲波长280 nm。结果:丹参素、原儿茶醛、橙皮苷、卅酚酸 B 进样浓度分别在7.0～223.0μg·mL~(-1)(r=0.9999),0.7～21.5μg·mL~(-1)(r=0.9999),8.5～272.0μg·mL~(-1)(r=0.9999),34.8～1112.0μg·mL~(-1)(r=0.9999)范围内呈良好的线性关系;平均回收率(n=6)分别为101.4%,98.9%,96.2%,99.4%及其 RSD 分别为2.4%,1.8%,1.3%,1.5%。结论:本方法简便,重现性好,结果准确可靠,为乳块消片的质量控制奠定了基础。     

毛细管气相色谱法测定无极膏中薄荷脑、樟脑、水杨酸甲酯、冰片及麝香草酚的含量

目的:建立 GC 法测定无极膏中薄荷脑、樟脑、水杨酸甲酯、冰片及麝香草酚含量的方法。方法:采用 HP-5弹性石英毛细管柱程序升温的方法测定。结果:5组分 GC 法测定的分离度和线性关系良好,薄荷脑、樟脑、水杨酸甲酯、冰片、麝香草酚线性范围分别为132.4～1324.0μg·mL~(-1),243.9-2439.0μg·mL~(-1),132.0～1320.0μg·mL~(-1),20.0～200.0μg·mL~(-1),10.1～101.3μg·mL~(-1);平均回收率分别为99.8%(RSD=0.9%),99.5%(RSD=1.2%),98.7%(RSD=0.9%),99.5%(RSD=1.2%),100.8%(RSD=1.6%)。结论:本法准确、灵敏,可用于该制剂的质量控制。     

HPLC法同时测定康复新液中两种成分的含量

目的:建立同时测定康复新液中尿苷和黄嘌呤含量的方法。方法:采用HPLC法,Diamonsil C18(250mm×4.6 mm,5μm)色谱柱,甲醇-水(5:95)作为流动相,于254 nm波长下检测,流速1.0 mL·min~(-1),柱温30℃。结果:尿苷、黄嘌呤分别在0.10~3.96μg·mL~(-1)(r~2=0.9998)、0.52~20.80μg·mL~(-1)(r~2=0.9992)浓度范围内线性关系良好,平均加样回收率分别为97.86%(RSD=1.25%)、97.39%(RSD=0.68%)。测定5批次康复新液中尿苷和黄嘌呤的含量范围分别为1.69~1.76μg·mL~(-1)、12.76~13.06μg·mL~(-1),说明各批样品质量较均一。结论:本文建立的方法精密度高、重复性好,操作简便快速,可用于康复新液的质量控制。     

HPLC法同时测定酚氨咖敏颗粒中三组分的含量

目的:建立 HPLC 法同时测定酚氨咖敏颗粒中对乙酰氨基酚、咖啡因、氨基比林的含量。方法:采用日本岛津 VP-ODS色谱柱(150 mm×4.6 mm,5μm),以甲醇-水(40:60)为流动相,流速:1.0 mL·min~(-1),检测波长273 nm,柱温:30℃,进样量:20 μL。结果:对乙酰氨基酚进样浓度在10～100μg·mL~(-1)范围内线性关系良好(r=0.9999),平均回收率(n=3)为98.8%～99.4%;咖啡因进样浓度在2.4～24μg·mL~(-1)范围内线性关系良好(r=0.9999),平均回收率(n=3)为98.2%～101.5%;氨基比林进样浓度在8～80μg·mL~(-1)范围内线性关系良好(r=0.9998),平均回收率(n=3)为98.3%～100.4%。结论:本方法灵敏度高,操作简便、可靠,适用于测定酚氨咖敏颗粒中对乙酰氨基酚、咖啡因、氨基比林的含量。     

Sirolimus and its analogs and its effects on vascular diseases

Sirolimus (rapamycin), a macrolide antibiotic approved for use as an immunosuppressive agent in the prevention of organ rejection, is a cell proliferation inhibitor and regulator of the immune response which acts through inhibition of TOR (target of rapamycin), a kinase essential to cell cycle progression. Recent studies suggest that the TOR pathway is critical to overall cell function, and at a basic mechanistic level, may be a regulator and potential therapeutic target involved in many of the major (and minor) disorders seen in man today. Cardiovascular diseases including restenosis following percutaneous coronary intervention as well as the more widespread condition of atherosclerosis, share this common involvement of TOR. The present report addresses the current state of intervention in cardiovascular disorders with Sirolimus and similar inhibitors of TOR, including the rationale for this approach and the successes observed to date. Success of the first drug-eluting stent to locally treat restenosis in the clinic is discussed, as are preclinical studies addressing a role in overall atherosclerosis in animal models. In addition, due to the known toxicities when given systemically, an approach for targeted delivery to local areas of vascular disease is discussed.     

Interaction of kynurenine and its metabolites with tryptamine,serotonin and its precursors and oxotremorine

Major metabolites of tryptophan: kynurenine (K), 3-hydroxykynurenine (3-HK), 3-hydroxyanthranilic (3-HAA), anthranilic (AA), picolinic (PA), quinolinic (QA) and nicotinic (NA) acids injected i.p. or s.c. were studied in rats and mice. In rats 3-HK, 3-HAA, AA and NA in doses of 5–20 mg/kg diminished 5-hydroxytryptophan-produced head-twitches but did not affect hypothermia. PA and NA also diminished tryptophan-produced head-twitches. In mice pretreated with nialamide the metabolites tested (3-HK and QA were not tested in a wide dose range) decreased tryptamine-produced head twitches and increased hyperthermia. K, 3-HAA, AA, PA and NA prolonged the latency of oxotremorine tremor in mice and did not influence hypothermia, salivation or diarrhoea.Antiserotonin and antitryptamine activity of metabolites of kynurenine could possibly enhance the deficiency of brain serotonin and tryptamine which occurs as a result of the tryptophan drain under emotional stress when corticosteroids activate liver tryptophan pyrrolase. Diminution of central serotoninergic and cholinergic processes by metabolites of K may be responsible for the shift of a balance between tropho- and ergotropic systems towards predominance of the ergotropic system.     

HPLC法测定大鼠血浆、微粒体中非那西丁与其代谢物含量及其应用

<正>细胞色素P450 1A2亚家族是近年来药物代谢研究领域的热点之一,与许多药物的相互作用有关[1]。非那西丁是CYP1A2酶的特异性底物,被广泛选择作为底物用于体内外测定酶活性[2]。本研究建立大鼠血浆、微粒体中非那西丁与其代谢物对乙酰氨基酚含量的HPLC测定方法,并对血浆样品进行方法学考察,为进一步确证药物及化学异物对CYP1A2酶活性的影响提供可靠的方法学基础。同时,应用所建立的方法以体内、体外方式评价了甘草水提液对     

羧甲基壳聚糖银的合成及抑菌实验的研究

目的研究羧甲基壳聚糖银的合成方法及其对金黄色葡萄球菌、铜绿假单胞菌、大肠埃希菌、肺炎克雷伯菌和变形杆菌的抑菌作用。方法对壳聚糖经化学修饰后的衍生物进行红外吸收光谱分析。用稀释法和凹环法对烧伤常见的病原菌进行抑菌实验。结果修饰后的衍生物经红外图谱分析表明 ,壳聚糖已被氯乙酸所修饰。羧甲基壳聚糖银对浓度均为 10 4 CFU/ml的金黄色葡萄球菌、大肠埃希菌、铜绿假单胞菌的抑菌率分别为 88%、80 .2 %和 75 .3%。羧甲基壳聚糖银和AgNO3 对金黄色葡萄球菌、铜绿假单胞菌的最低抑菌浓度相同 ,对大肠埃希菌的最低抑菌浓度则前者低于后者。结论羧甲基壳聚糖银对烧伤感染常见致病菌有抑制作用 ,它可作为一种新型的预防、治疗烧伤感染的药物。     

加替沙星制剂中有关物质检查与含量测定的高效液相色谱法

目的　建立加替沙星制剂中加替沙星的含量及其有关物质测定的 RP- HPL C法。方法　采用Shimpack VP- ODS柱 (15 0 mm× 4 .6 mm,5 μm) ,流动相为 1%三乙胺 (磷酸调节 p H至 4 .5 ) -乙腈 (82∶ 18,体积比 ) ,检测波长 32 5 nm。结果　加替沙星在 2 .32～ 4 6 .4 8μg/ ml浓度范围内线性关系良好 ,日内及日间 RSD分别为 1.1%和 1.7%。平均回收率为 99.9% ,RSD为 0 .6 5 %。最低检测限为 0 .2 μg/ ml。结论　该方法简单 ,灵敏度高 ,结果准确 ,可用于加替沙星制剂的含量测定及有关物质检查。     

Nicotine, its metabolism and an overview of its biological effects.

Nicotine is a naturally occurring alkaloid found in many plants. The principal sources of nicotine exposure is through the use of tobacco, nicotine containing gum and nicotine replacement therapies. Nicotine is an amine composed of pyridine and pyrrolidine rings. It has been shown that nicotine crosses biological membranes and the blood brain barrier easily. The absorbed nicotine is extensively metabolized in the liver to form a wide variety of metabolites including nicotine N'-oxide and cotinine N'-oxide. These are the products of mixed function oxidase system. Nicotine is also converted to some biologically important compounds during harvesting. Among these are the nitrosamines specific to tobacco. Nicotine has been shown to affect a wide variety of biological functions ranging from gene expression, regulation of hormone secretion and enzyme activities. The objective of this study was to overview the biological effects and metabolism of nicotine.     

HPLC-MS法同时测定人血浆中氯沙坦及其代谢物EXP3174

目的:建立人血浆中氯沙坦及其代谢物EXP3174同时测定的HPLC-MS方法,并研究健康受试者单剂量口服氯沙坦钾片后氯沙坦及其代谢物EXP3174的药代动力学特征. 方法:血浆样品以乙腈沉淀蛋白后,进行HPLC-MS分析,色谱柱为Lichrospher C18,流动相为甲醇-20 mmol·L-1醋酸铵水溶液(含0.1 %的甲酸)(60:40,V/V),氯沙坦及其代谢物EXP3174的检测离子均为m/z 207.1,传输区电压为250 V.12名男性健康受试者口服100 mg氯沙坦钾片后,测定血浆中氯沙坦及其代谢物EXP3174的浓度,计算主要药动学参数.结果:在1～2000 ng·mL-1范围内,氯沙坦及其代谢物EXP3174两者峰面积与内标峰面积的比值和浓度的线性关系均良好,批内、批间RSD均小于10%.受试者口服100 mg氯沙坦钾片后,氯沙坦的血药浓度达峰时间为(1.6±1.1)h,达峰浓度为(890.2±476.4)ng·mL-1,消除半衰期为(2.7±1.6)h;EXP3174的血药浓度达峰时间为(2.9±1.0)h,达峰浓度为(1233±611.6)ng·mL-1,消除半衰期为(6.4±1.2)h.结论:本试验通过选择相同的碎片离子作为氯沙坦及其代谢物EXP3174的检测离子,提高了灵敏度和准确度;所建立的HPLC-MS分析方法准确、灵敏、方便,可用于氯沙坦及其代谢物的人体药动学研究.     

Antidiabetic activity of Aegle marmelos and its relationship with its antioxidant properties

Oxidative stress induced by alloxan has been shown to damage pancreatic beta-cell and produce hyperglycemia in rats. Aegle marmelos leaf extract is being used in Ayurveda as a medicine for diabetes. The present study examined the action of Aegle marmelos against experimental diabetes as well as the antioxidant potential of the drug. A methanolic extract of Aegle marmelos was found to reduce blood sugar in alloxan diabetic rats. Reduction in blood sugar could be seen from 6th day after continuous administration of the extract and on 12th day sugar levels were found to be reduced by 54%. Oxidative stress produced by alloxan was found to be significantly lowered by the administration of Aegle marmelos extract. This was evident from a significant decrease in lipid peroxidation, conjugated diene and hydroperoxide levels in serum as well as in liver induced by alloxan. Catalase and glutathione peroxidase activity in blood and liver were found to be increased from 9th day onwards after drug administration. Superoxide dismutase and glutathione levels were found to be increased only on 12th day. These results indicate that Aegle marmelos extract effectively reduced the oxidative stress induced by alloxan and produced a reduction in blood sugar.