RP-HPLC法测定复方氧氟沙星鱼肝油乳剂中氧氟沙星和甲硝唑的含量

目的:建立反相高效液相色谱法测定复方氧氟沙星鱼肝油乳剂中甲硝唑和氧氟沙星的含量.方法:采用反相高效液相色谱法,色谱柱为Diamonsii C18柱(250mm×4.6mm,5μm), 流动相为甲醇-1%醋酸铵(40∶60),流速1.0mL·min-1, 检测波长293nm.结果:甲硝唑在3.0～30.0μg·mL-1范围内线性关系良好,回归方程:Y=0.123 30 1.833 75X,r=0.999 9(n=5),平均回收率100.33%,RSD=1.49%(n=9);氧氟沙星在2.0～20.0μg·mL-1范围内线性关系良好,回归方程:Y=0.157 53 0.623 53X,r=0.999 9(n=5),平均回收率100.31%,RSD=1.19%(n=9).结论:该方法灵敏度高;专属性好;操作简便;重现性好.     

高效液相色谱法测定复方甲硝唑乳膏中甲硝唑和乳酸环丙沙星的含量

目的:建立复方甲硝唑乳膏中甲硝唑和乳酸环丙沙星含量测定的HPLC法.方法:采用Waters Symmetry C18色谱柱(250 mm×4.6 mm,5 μm),流动相为0.05 mol·L-1枸橼酸(三乙醇胺调pH至3.5)-乙腈(82:18),检测波长为287 nm,流速为1.0 ml·min-1.结果:甲硝唑浓度在20.0～100.0 μg·ml-1范围内与峰面积呈良好的线性关系(r=0.999 9),平均回收率为98.3%RSD为0.7%(n=5);乳酸环丙沙星浓度在16.0～80.0 μg·ml-1范围内与峰面积呈良好的线性关系(r=0.999 9),平均回收率为98.6%,脚%为0.9%(n=5).结论:方法简便、快捷,结果准确,适用于该制剂的质量控制.     

食用植物油中残留溶剂的气相色谱分离与测定

目的建立食用植物油中正己烷、环己烷残留量的含量测定方法。方法样品用N,N-二甲基甲酰胺溶解后,利用气相色谱法,顶空进样对样品进行测试。结果正己烷质量浓度(X)在5.260¹57.8mg·L-1范围内与峰面积积分值(Y)回归线性方程:Y=0.412 2 X+1.294 8,r=0.999 8,线性关系良好;环己烷质量浓度(X)在4.218157.8mg·L-1范围内与峰面积积分值(Y)回归线性方程:Y=0.412 2 X+1.294 8,r=0.999 8,线性关系良好;环己烷质量浓度(X)在4.218¹26.5mg·L-1的范围内,与峰面积积分值(Y)回归线性方程:Y=0.257 5 X+0.857 3,r=0.999 8,线性关系良好;平均回收率正己烷为99.0%,RSD为0.6%;环己烷为98.8%,RSD为0.8%。结论该方法准确、可靠、简便,可用于测定食用植物油中正己烷和环己烷残留量的检测。     

超高效液相色谱法测定半夏不同炮制品中核苷类成分含量

目的建立以超高效液相色谱(UPLC)法测定不同炮制工艺半夏中尿苷、鸟苷和腺苷含量的方法。方法色谱柱为ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7μm),流动相为水-甲醇,梯度洗脱,柱温30℃,流速0.5 m L·min-1,检测波长254 nm。结果尿苷在2.214~22.140μg·m L-1浓度范围内线性关系良好,回归方程为:Y=93 991X-1 653(r=0.999 9),平均回收率为99.18%,RSD=2.40%;鸟苷在1.212~12.120μg·m L-1浓度范围内线性关系良好,回归方程为:Y=61 542X-806(r=0.999 9),平均回收率为98.88%,RSD=1.16%;腺苷在0.245 2~2.452 0μg·m L-1浓度范围内线性关系良好,回归方程为:Y=14 994X-145(r=0.999 9);平均回收率为98.66%,RSD=0.97%。结论该方法准确、快速,能有效地测定不同炮制工艺半夏中尿苷、鸟苷和腺苷的含量。     

高效液相色谱法测定复方林氯滴眼液中盐酸林可霉素的含量

目的建立HPLC法测定复方林氯滴眼液中盐酸林可霉素的的含量.方法采用BDS C18色谱柱(250 mm×4.6 mm,5 μm),以0.05 mol·L-1硼砂溶液(用磷酸调节pH值至 6.0)-甲醇(2∶3)为流动相,流速1 ml·min-1,紫外检测波长为214 nm.结果林可霉素的峰面积与浓度呈良好的线性关系,线性范围为0.2～2.0 g·L-1,回归方程Y=2.003×106X 1.445×104(r=0.999 9,n=5).回收率为99.4%,RSD=0.40%.分析方法精密度RSD为1.26%(n=5).结论该方法简便、快速、准确.     

高效液相色谱法测定黄藤素片中盐酸巴马汀的含量

目的: 建立高效液相色谱法测定黄藤素片中盐酸巴马汀的含量.方法: 色谱柱为Diamonsil ODS C18 柱(200 mm×4.6 mm, 5 μm).流动相为乙腈-缓冲液(0.05 mol·L-1磷酸二氢钾和0.05 mol·L-1 庚烷磺酸钠,1: 1)(50: 50),检测波长272 nm,流速:0.8 ml·min-1,柱温:室温.结果: 盐酸巴马汀在8.032～40.160 μg·ml-1范围内浓度与峰面积呈良好的线性关系,回归方程Y=1.01×104X 7.86×104, r=0.999 6,平均回收率为99.5%,RSD为1.0%(n=9).结论: 本法简便、灵敏、准确,可作为该制剂的定量分析方法.     

HPLC法测定复方醋酸棉酚片中维生素B1和B6的含量

目的建立高效液相法同时测定复方醋酸棉酚片中维生素B1和B6含量的方法。方法采用C18(150 mm×4.6 mm,5μm)色谱柱;流动相:庚烷磺酸钠溶液(取庚烷磺酸钠0.4 g,加三乙胺3 mL,加水至1 000 mL,用磷酸调pH值至3.5)-甲醇(75∶25);流速:1.0 mL.min-1;检测波长:275 nm。结果维生素B1在10.05～200.92 mg.L-1质量浓度范围内与峰面积呈良好的线性关系Y=13 744.72X+44 526.49(r=0.999 9),回收率为99.4%,RSD=1.1%(n=9)。维生素B6在10.43～208.60 mg.L-1质量浓度范围内与峰面积呈良好的线性关系Y=120101.31X-14766.07(r=0.999 9),回收率100.1%,RSD=1.2%(n=9)。结论该方法简便、准确,可同时测定复方醋酸棉酚片中维生素B1和B6的含量。     

高效液相色谱法同时测定复方8-甲氧补骨脂素洗剂中主药含量

目的:建立复方8-甲氧补骨脂素洗剂中复方8-甲氧补骨脂素和醋酸肤轻松含量测定的高效液相色谱法.方法:采用Waters Symmetry C18色谱柱(250mm×4.6mm,5μm),流动相为甲醇-水(70:30),检测波长为240nm,流速为1.0ml·min-1.结果:8-甲氧补骨脂素浓度在20.232～101.16mg·L-1范围内与峰面积呈良好的线性关系(r=0.9999),平均回收率为100.70%(RSD为0.82%).醋酸肤轻松浓度在5.232～26.16 mg·L-1范围内与峰面积呈良好的线性关系(r=0.9998),平均回收率为100.8%(RSD为1.11%).结论:本法简便、快捷,结果准确,适用于该制剂的质量分析检验.     

HPLC法同时测定人血清中万古霉素和去甲万古霉素浓度

目的:建立人血清中万古霉素和去甲万古霉素浓度的HPLC测定方法.方法:色谱柱为Hypersil BDS C18 (250mm×4.6mm,5μm)柱;流动相为磷酸二氢钾缓冲液-甲醇(85:15),流速1ml·min-1;检测波长236nm;以甲硝唑为内标,采用高氯酸直接沉淀蛋白后进样.结果:万古霉素、去甲万古霉素血清浓度与峰面积线性关系良好,万古霉素回归方程为Y=0.0106+0.0202X,r=0.999 7;去甲万古霉素回归方程为Y=-0.0164+0.0286X,r=0.999 9;线性范围2.0～100.0mg·L-1.日内RSD小于7.2%,日间RSD小于6.9%;万古霉素高、中、低浓度的平均方法回收率分别为97.73%,97.58%,103.91%,平均提取回收率分别为86.80%,85.50%,87.63%;去甲万古霉素高、中、低浓度的平均方法回收率分别为100.23%,92.63%,97.57%,平均提取回收率分别为90.84%,87.82%,89.68%.结论:方法操作简便快速,回收率稳定,适于临床血药浓度测定及相关科研的应用.     

LPLC法同时测定复方甲硝唑软膏中甲硝唑和氯霉素的含量

目的:建立复方甲硝唑软膏中甲硝唑和氯霉素的含量测定方法,方法:采用高效液相色谱法,色谱柱为VP-ODS色谱柱(150 mm×4.6 mm,5μm);流动相:甲醇-水(30∶70);流速:1.0 ml/min;柱温:30℃;检测波长:277 nm。结果:甲硝唑进样量在0.02~0.16 mg/ml范围内线性关系良好,回归方程为Y=5.515 7×10-8X-1.997 9×10-3,r=0.999 9,平均回收率为99.96%,RSD为0.12%(n=9);氯霉素进样量在0.01~0.15 mg/ml内线性关系范围,回归方程为Y=2.811 1×10-8X-5.875 6×10-4,r=0.999 8,平均回收率为101.07%,RSD为0.55%(n=9)。结论:测定方法简便、准确、重现性好,适于复方甲硝唑软膏的含量测定。     

阿昔洛韦药物树脂的制备

目的:制备阿昔洛韦药物树脂复合物并对影响因素(温度、流速、粒径、浓度)进行考察。方法:静态交换法和动态交换法。结果:静态制备的优化条件是温度25℃,药物浓度7 mg·mL-1,树脂粒径60—80μm;动态制备的优化条件是温度25℃,药物浓度7．5 mg·mL-1,树脂粒径100-120μm,流速2 mL·min-1。结论:难溶性药物阿昔洛韦可制成药物树脂,且采用静态交换法制备树脂较好。     

阿昔洛韦胃漂浮片的制备

目的研制阿昔洛韦胃漂浮片。方法采用粉末直接压片法制备阿昔洛韦胃漂浮片,以漂浮性能和阿昔洛韦的释放度为考察指标进行处方筛选。结果以羟丙基甲基纤维素(HPMC K4M)和聚氧乙烯(PEO WSR N-205)为亲水凝胶骨架,十六醇为助漂剂,碳酸氢钠为产气剂,制备了12 h缓释胃漂浮片。该制剂在胃酸中立即起漂,2 h释放30%,6 h释放60%,12 h释放大于90%。结论所制备的阿昔洛韦胃漂浮片具有良好的漂浮性和缓释特性。     

阿昔洛韦致过敏性休克

1例34岁女性患者因带状疱疹自行涂抹3%阿昔洛韦软膏及自行静脉滴注阿昔洛韦0.25 g+0.9%氯化钠注射液100 ml。滴注约2 min后患者出现口唇麻木、胸部不适、头晕、乏力,立即停药,急诊入院,给予吸氧。旋即患者头面部、胸部及四肢近端皮肤出现红斑,口唇发绀、肿胀。停药约8 min患者出现视物不清,血压降至70/40 mm Hg(1 mm Hg=0.133 kPa)。约13 min出现黑曚、恶心、呕吐。经静脉注射地塞米松和肾上腺素、静脉滴注氢化可的松以及泵入多巴胺和去甲肾上腺素等处理,14 h后患者过敏症状完全消失。     

Evaluation of oral acyclovir therapy

Acyclovir is a specific antiviral agent. The triphosphate form inhibits viral DNA replication by competing for incorporation into the replicating DNA chain or by inhibiting viral DNA polymerase. Cells not infected with herpesvirus are generally unaffected. Oral acyclovir inhibits most herpes simplex virus types 1 and 2, and varicella-zoster virus at concentrations used clinically. Oral acyclovir has an average plasma half-life of three hours and is eliminated primarily by renal mechanisms. Peak plasma concentrations occur 1.5 to 2.5 hours after administration and the oral bioavailability is 15 to 30 percent. Acyclovir distributes into most body tissues, including vesicular fluid and the central nervous system. Oral acyclovir is effective treatment of initial and recurrent genital herpes and can suppress frequently recurring genital herpes in both immunocompetent and immunocompromised patients. It is also effective for acute herpes zoster in the immunocompetent and possibly immunocompromised patient. No role is established in either Epstein-Barr virus or cytomegalovirus infections. Oral acyclovir appears to be effective and relatively safe, nontoxic therapy when administered in doses of 1-4 g/d. Oral acyclovir represents a major therapeutic advance in the treatment of herpesvirus infections.     

Polymorphism and pseudopolymorphism of acyclovir

Four crystal modifications of acyclovir were isolated by recrystallization and characterized by powder X-ray diffractometry, differential scanning calorimetry, and thermogravimetric analysis. It was confirmed that Form 3 is a hydrate and Form 4 is an acetic acid solvate. The dissolution patterns of three crystal forms of acyclovir were studied in water at 37±0.5°C, 90 rpm for 120 minutes. The amount dissolved at 120 minutes was highest for Form 1, followed by Form 2 and Form 3. After storage of 25 hours at 0% RH (silica gel, 20°C) Form 3 was transformed to Form 2.     

口服阿昔洛韦片的相对生物利用度

目的观察两种阿昔洛韦片剂的人体相对生物利用度。方法9名健康志愿者随机交叉口服单剂量400mg 仙居产或丽珠产阿昔洛韦片后 ,采用HPLC法测定不同时间血药浓度 ,并计算生物利用度参数。结果仙居与丽珠产阿昔洛韦片主要生物利用度参数均值分别为 :Tp为1.6和1.7h,AUC为3.496和3.693μg/ml·h,Cmax 为1.011和0.997μg/ml,MRT为3.27和3.53h。结论经双向单侧检验法分析表明仙居与丽珠产阿昔洛韦片剂生物等效。     

Polymorphs and hydrates of acyclovir

Acyclovir (ACV) has been commonly used as an antiviral for decades. Although the crystal structure of the commercial form, a 3:2 ACV/water solvate, has been known since 1980s, investigation into the structure of anhydrous ACV has been limited. Here, we report the characterization of four anhydrous forms of ACV and a new hydrate in addition to the known hydrate. Two of the anhydrous forms appear as small needles and are stable to air exposure, whereas the third form is morphologically similar but quickly absorbs water from the atmosphere and converts back to the commercial form. The high-temperature modification is achieved by heating anhydrous form I above 180 °C. The crystal structures of anhydrous form I and a novel hydrate are reported for the first time.     

Prenatal toxicity of acyclovir in rats

Pregnant rats were treated during organogenesis with s.c. injections of acyclovir and the embryos were evaluated on day 11.5 of gestation (crown-rump length, somites, protein content, score, abnormalities, histological examination). After eight injections of 50 mg/kg body wt on days 9, 10, and 11 of pregnancy a reduction of the crownrump length was noticed. After 100 mg/kg this effect was more pronounced. With two or three applications of this dose on day 10 specific embryonic abnormalities were visible: the shape of the head was abnormal, the width of the skull had decreased resembling a beak-like visceral cranium. With a single administration of 200 mg/kg on day 10 we found a similar but slightly more pronounced outcome. A drastic change of all variables was obtained after eight injections of 100 mg/kg on days 9, 10, and 11. Comparatively we measured maternal plasma concentrations of acyclovir 1 h after the administration of 50, 100 or 200 mg/kg body wt. After an injection of 50 mg/kg on days 9, 10, and 11 of gestation (three injections/day) the plasma levels ranged from 19.1 to 40.0 mg/l (1 mg/l = 4.44 M). No cumulation was observed. In contrast, a cumulative effect was detected following a dose of 100 mg/kg. After the first injection of this dose a mean value (± SD) of 60.3±14.7 mg/l (n = 16) was obtained. In this case a third injection increased the mean plasma level to 124.6±16.6 mg/l (n = 5). Further injections, however, led to decreasing levels. One hour after administration of 200 mg/kg body wt acyclovir levels ranged from 120.0 to 163.9 mg/l. We conclude that acyclovir, at doses leading to plasma concentrations well above the therapeutic level in the dam, interferes with the embryonic development in the rat. Acyclovir induces typical gross structural abnormalities which have been first observed using a whole embryo culture system.     

Topical delivery of acyclovir and ketoconazole

Abstract

Context: Viral and fungal cutaneous manifestations are regularly encountered in immunocompromised human immunodeficiency virus/acquired immunodeficiency syndrome individuals and can be treated by drugs such as acyclovir and ketoconazole, respectively.

Objective: The aim of this study was to determine whether the novel Pheroid? delivery system improved the transdermal delivery and/or dermal delivery of acyclovir and ketoconazole when incorporated into semi-solid formulations.

Materials and methods: Semi-solid products (creams and emulgels) containing these drug compounds were formulated, either with or without (control) the Pheroid? delivery system. The stability of the formulated semi-solid products was examined over a period of six months and included the assay of the actives, pH, viscosity, mass loss and particle size observation. Vertical Franz cell diffusion studies and tape stripping methods were used to determine the in vitro, stratum corneum (SC)-epidermis and epidermis-dermis delivery of these formulations.

Results and discussion: Stability tests showed that none of the formulations were completely stable. Acyclovir showed a biphasic character during the in vitro skin diffusion studies for all the tested formulations. The Pheroid? cream enhanced the transdermal, SC-epidermis and epidermis–dermis delivery of acyclovir the most. The average amount of ketoconazole diffused over 12?h showed improved delivery of ketoconazole, with the Pheroid? emulgel exhibiting the best transdermal and epidermis–dermis delivery.

Conclusion: The Pheroid? formulae increased transdermal penetration as well as delivery to the dermal and epidermal skin layers. The Pheroid? emulgel and the Pheroid? cream increased the topical delivery of ketoconazole and acyclovir, respectively.