HPLC法测定环孢素胶丸的含量

报道了环孢素胶丸的高效液相色谱测定法。固定相为H_5ODSC_(-18),乙醇-水(60:40,v/v)作流动相。检测波长UV210nm,线性范围10～400μg/ml(r=0.9995),回收率98.2％(n=6)。此法快速、准确的测定胶丸中环孢素含量,且辅料无干扰,测定差异小。     

HPLC法测定人血清中头孢呋肟浓度

本文建立了快速、简便测定人血清中头孢呋肟反相HPLC法,采用5×20mn不锈钢柱内填10um YWG-C_(18)H_(37)17定相,流动相甲醇:水:冰醋酸(28:71:1v/v),流速1.2ml/min,以头孢噻肟为内标物,紫外检测波长290nm,用10％三氯醋酸作蛋白沉淀剂,与血清之比为1:2(v/v)。头孢呋肟的日内回收率为100.34±6.60％,日间回收率为99.69±6.33％。头孢呋肟最低检测限为2ng,最低检测浓度为0.2μg/ml。在0.25～10μg/ml浓度范围内线性良好,相关系数r=0.9999。     

反相HPLC法测定油剂中的睾酮酯类

睾酮酯的测定通常采用分光光度法,但该法对油性注射剂专一性不强,由于抑菌剂苯甲醇氧化后生成的苯甲醛及油剂本身均产生干扰,因此作者研究了HPLC法测定油剂中的睾酮酯类.HPLC条件:层析柱为Lichrosorb RP-8(250×4mm,id),流动相A为甲醇-四氢呋喃-水(82∶3∶15v/v),用于苯丙酸诺龙,以联苯作内标;流动相B为甲醇-四氢呋喃-水(90∶2∶8v/v),用于睾酮癸酸酯     

羧(艹卡)青霉素和替卡西林注射剂的液相色谱测定

本文报道了应用反相液相色谱法测定注射剂中的羧苄青霉素(carbenicillin)和替卡西林(ticarcillin,羧噻吩青霉素)。该法选用ODS不锈钢色谱柱(30cm×3.9mm),以含有0.01mol/L乙腈的磷酸二氢钾(12+88v/v)为流动相,在225nm处检测。用丙硫脲作内标。     

复方石韦片中绿原酸在大鼠血浆中的测定及药代动力学研究

目的 建立了高效液相色谱法测定大鼠血浆中绿原酸的含量及其在大鼠体内的药物动力学研究.方法 色谱条件采用Diomonsil C18反相柱(4.6mm×250mm,5μm),以乙腈-0.5％磷酸溶液(10∶90,v/v)为流动相,柱温为35℃,流速为1.0mL · min -1,检测波长为360nm,进样量为10μL.结果...     

HPLC法测定异环磷酰胺血药浓度方法的改进

目的建立以甲醇-水为流动相测定异环磷酰胺血药浓度的方法,以降低治疗药物监测的成本.方法用氯仿萃取血清中的异环磷酰胺,浓集后进样测定.在室温条件下,使用ELITE C18色谱柱(250 mm×4.5 mm,5μm),以甲醇-水(1:1,v/v)为流动相,以咖啡因为内标,检测波长200 nm.结果本方法线性范围10～200 mg·L-1,相关系数0.999 2,最低检测浓度5.2 mg·L-1,回收率94%～103%.结论该方法灵敏度较高、准确度较好、操作简便,适用于对异环磷酰胺进行治疗药物监测,并且成本较低.     

高效液相色谱法检查盐酸洛美利嗪片有关物质

目的:建立高效液相色谱法测定盐酸洛美利嗪片中有关物质的测定方法,以控制其质量。方法:采用高效液相色谱法Shimadzu Vp-ODS C18柱,以甲醇-乙腈-15mol.L-1磷酸二氢钠(pH7.5,2∶2∶1,v/v)为流动相;检测波长220nm。结果:该方法对各种分解产物分离良好,检测限为10ng。结论:该方法简便、快速,适用于盐酸洛美利嗪片中有关物质的检查。     

应用加压毛细管电色谱技术检测鸡蛋中四环素类农兽药残留的研究

目的 建立了鸡蛋样品中四环素类农药多残留同时检测的加压毛细管电色谱分析方法。方法 以二氯甲烷为沉淀剂处理鸡蛋样品,运用加压毛细管电色谱法进行快速检测。以甲醇-乙腈-20 mmol/L草酸溶液(pH=4.25)(10：20：70,v/v/v)作流动相,等度洗脱,外加电压为-4kV,检测波长为270 nm。结果 经方法学考察,4种四环素类药品土霉素、4-差向金霉素、盐酸金霉素、强力霉素在各自标准曲线浓度范围内线性良好,R2均在0.993以上。回收率为80.46％～100.49％,日内和日间精密度的相对标准偏差(RSD)均低于5％。结论 该方法简单方便,重现性好,准确可靠,回收率较高,适用于鸡蛋样品中抗生素多残留的测定。     

葛根素中4′-甲氧基葛根素的反相高效液相色谱法测定(英文)

本文报道应用反相高效液相色谱法测定葛根素中4′-甲氧基葛根素的含量,以对羟基苯甲醛作内标,在填充以LiChrosorb RP-18(10μm)固定相的不锈钢柱上,以EtOH-H_2O(10:90)作流动相,检测波长为250nm。本法与TLC-UV法比较,测定结果一致,但本法简便、快速、重现性好,可以应用於葛根素原料药及其制剂中葛根素和4′-甲氧基葛根素的含量测定。     

反相高效液相色谱法测定乙酰麦迪霉素血药浓度

应用反相高效液相色谱法测定乙酰麦迪霉素血清浓度。色谱柱为ODS O₁₈柱,流动相为甲醇一水(80:20,v/v),流速1.0 ml/min,检测波长254 nm,柱温25℃。线性范围在10～300 ng/ml,检测下限为10 ng/ml 高、低浓度平均回收率分别为101.02%和105.44%,日内,日间测定RSD 分别为5.12%(n=10)和7.38%(n=7)。应用本法测定健康人单剂量日服乙酰麦迪霉素干糖浆后的血药浓度,结果满意。     

紫杉醇生产新工艺研究

从红豆杉茎皮提取紫杉醇，采用１％柠檬酸渗漉、柱色谱分离、溴加成后柱色谱分离的新工艺，可以获得比较满意的结果。     

红豆杉中紫杉醇的高效液相色谱法测定(英文)

本文研究了高效液相色谱法测定红豆杉Taxus chinensis中紫杉醇的含量,以倍他米松作内标,在填充以YWG 80(10μm)固定相的不锈钢色谱柱上,以CH₂Cl₂-MeOH(95:5)作流动相,在UV 228 nm波长进行检测,其变异系数小于2%。     

南方红豆杉与引种德国曼地亚红豆杉茎、叶中紫杉醇和10-脱乙酰巴卡亭Ⅲ含量的比较

目的建立HPLC法同时测定并比较南方红豆杉与德国引种曼地亚红豆杉茎、叶中紫杉醇和10-脱乙酰巴卡亭Ⅲ含量。方法采用Cosmasil TMC18色谱柱(250mm×4.6mm,5μm);以乙腈-水(50∶50)为流动相;流速为1.0mL·min-1;检测波长为227nm;柱温:30℃。结果紫杉醇、10-脱乙酰巴卡亭Ⅲ的线性范围分别为2.675⁴2.8μg·mL-1(r=0.999 3)和3.87542.8μg·mL-1(r=0.999 3)和3.875⁶2μg·mL-1(r=0.999 6),平均加样回收率(n=9)分别为98.1%和101.6%,RSD分别为2.7%和2.3%。南方红豆杉与德国引种曼地亚红豆杉的茎、叶中紫杉醇含量分别为0.12和0.10mg·g-1,10-脱乙酰巴卡亭Ⅲ含量分别为0.12和0.14mg·g-1。结论引种红豆杉与南方红豆杉在同一地区的生态环境下生长,茎、叶中所含紫杉醇和10-脱乙酰巴卡亭Ⅲ含量有显著性差异(P<0.05)。所建立方法准确,简便,适用于红豆杉的质量评价,为不同栽培品种的选择提供参考。     

HPLC法测定南方红豆杉种子中紫杉醇的含量

目的:建立高效液相色谱测定南方红豆杉种子中紫杉醇含量的方法.方法:采用Whatman C18 (250 mm × 4.6 mm,5.0 μm) 色谱柱,柱温30℃;流动相为乙腈-水(35∶65-80∶20)30 min梯度洗脱,流速1.0 mL/min;检测波长227 nm.结果:紫杉醇的线性范围:8.5 ~ 51.0...     

紫杉醇的半合成

以红豆杉属植物枝叶中含量丰富且易于提取的10-去乙酰-bacatinII(I)为原料,通过区域选择性反应得到被保护的紫杉醇母核;以α-甲基-苯甲胺为Staudinger反应的手性辅助剂,经7步反应合成了被保护的紫杉醇侧链(4S,5R)-N-(叔丁氧甲酰基)-2,2-二甲基-4-苯基-1,3-氧氮杂环戊烷-5-甲酸(X);以DCC为缩合剂连接侧链与母核,进而成功地半合成得到紫杉醇(I)。该途径可能是缓解紫杉醇供应危机的可行手段之一。     

湘产南方红豆杉中紫杉醇含量动态变化的研究

目的掌握湘产南方红豆杉不同生长季节的枝叶中紫杉醇含量的动态变化规律,确定最佳采收期。方法高效液相色谱法对湘产南方红豆杉不同生长季节的枝叶中紫杉醇含量进行了测定和分析。结果从3月新枝叶萌发至6月份紫杉醇的含量逐渐增加,6月份枝叶中紫杉醇含量最高,7月份开始紫杉醇的含量逐渐减少。结论6月份为湘产南方红豆杉枝叶的最佳采收期。     

Enzyme-linked immunosorbent assay for the detection and the semi-quantitative determination of taxane diterpenoids related to taxol in Taxus sp. and tissue cultures.

An ELISA-assay for the detection and the semi-quantitative determination of taxane diterpenoids structurally related to taxol found in Taxus sp. has been developed. The antiserum was raised in rabbits using a 2'-succinyltaxol-bovine serum albumin conjugate as immunogen. The working range of the assay was from 1 to 100 ng of taxol. In order to improve the production of taxol, preliminary experiments have been performed on crude extracts of several Taxus sp.; the results indicate that the present immunoassay is an useful tool for the rapid screening of species, varieties or individual plants out of a large population as well as for tissue cultures analysis.     

High sensitivity ELISA determination of taxol in various human biological fluids

Taxol (paclitaxel)--the natural product isolated from Pacific yew (Taxus brevifolia)--is a novel agent with high activity in the treatment of patients with several malignant tumors including those resistant to other cytotoxic drugs. The therapeutic index of this promising anticancer drug could be further increased by the exploration of its pharmacokinetic pharmacodynamic relationship in cancer patients. Since taxol is highly protein bound, a very specific and highly sensitive analytical method is required in order to determine free, protein unbound and biologically active taxol species in human physiological fluids: plasma; plasma ultrafiltrate; and salivary fluids. In order to accomplish this, a new indirect competitive enzyme-linked immunosorbent assay (ELISA), for quantitating such a low bioactive taxol concentration level, has been developed in our laboratories. This method uses taxol competitive inhibition of mouse anti-taxol antibodies binding to the solid phase coated antigen 7-succinyltaxol-bovine serum albumin. This indicates recognition of the active taxol in the solution phase, where a diluted horseradish peroxidase labeled goat anti-mouse enzyme conjugate is used. While employing this technique, after systematic optimization of the experimental conditions, we are able to detect the anticipated taxol in plasma ultrafiltrate and salivary fluids at the concentration level of subpicogram per milliliter. The working range of the assay is approximately five orders in magnitude, i.e. from pg ml(-1) to 100 ng ml(-1). The clinical part of this study verified the working range of the ELISA method using samples of physiological fluids from a cancer patient treated with 3 h intravenous (i.v.) infusion of this drug. Our results of taxol determination in plasma, plasma ultrafiltrate and saliva demonstrate the applicability of the newly developed ELISA method for further pharmacokinetic studies of free, biologically active taxol species in cancer patients.     

紫杉醇注射液在大鼠体内的药代动力学研究

目的建立测定大鼠血浆中紫杉醇的高效液相色谱（HPLC）法，并研究紫杉醇注射液在大鼠体内的药代动力学。方法8只SD大鼠单剂量尾静脉给药，采用HPLC法测定紫杉醇的血药浓度，采用DAS药动学程序对经时血药浓度进行室模型拟合和分析。结果从零时至所有原形药物全部消除时的药-时曲线下总面积（AUC0→∞）为（19．9636±9．6893）mg／（L·h），分布相半衰期（t1／2α）为（0．2055±0．2213）h，消除相半衰期（t1／2β）为（1．0786±0．3280）h，清除率（CL）为（0．3438±0．1111）L／（h·kg），中央室表观分布容积（Vd）为（0．2009±0．1280）L／kg。结论HPLC法简便、灵敏，可用于紫杉醇的血药浓度测定；紫杉醇在大鼠体内的处置符合二室模型。     

Novel taxane derivatives from Taxus wallichiana with high anticancer potency on tumor cells

Four novel taxane derivatives, N‐debenzoyl‐N‐methyl‐N‐heptanoyl‐taxol ( 1 ), N‐debenzoyl‐N‐me‐thyl‐N‐octanoyl‐taxol ( 2 ), N‐debenzoyl‐N‐methyl‐N‐(4‐methylhexanoyl)‐taxol ( 3 ), and N‐debenzoyl‐N‐methyl‐N‐[(4Z)‐1‐oxo‐4‐tenenoyl]‐taxol ( 4 ), were isolated from the ethanol extract of the whole plant of Taxus wallichiana.var.mairer. These structures were identified on the basis of extensive spectroscopic analysis, and their antitumor activity was evaluated against MCF‐7, A549, and 3‐AO cancer cell lines by the MTT method. Compound 3 , the most promising one, exhibited encouraging effect with IC₅₀ of 77 nm in MCF‐7 cells, which was almost matching that of positive control Taxol. In further mechanism study, the tubulin polymerization assay demonstrated that four compounds caused shifts from the soluble tubulin (depolymerized tubulin) to the particulate tubulin fraction (polymerized) which was similar to Taxol. These results revealed novel natural products with paclitaxel‐likemicrotu‐bule‐stabilizing activity owned their major importance in the clinical treatment of cancer.