罗红霉素电子药膜的研制及其稳定性考察

目的 :制备罗红霉素电子药膜 ,建立测定罗红霉素电子药膜含量的方法 ,考察其膜剂稳定性。方法 :采用电热成膜法制备膜剂 ;含量测定采用高效液相色谱法 ,色谱柱为YWG -C18柱 ,流动相为乙腈 -甲醇 -0 .5 %乙酸铵 ( 10 0 80 60 ) ,检测波长为 2 35nm ;稳定性实验 ,采用 4 0℃、60℃、80℃为考察温度 ,以相对湿度 75 % (NaCl)和 92 .5 % (KNO3 )为考察湿度 ,于第 0、1、3、5、10d时取样测定罗红霉素含量。结果 :每片膜剂含罗红霉素 75mg ,重量差异限度小于 10 % ;高效液相色谱法加样回收率高 ,在 0 .3～ 1.7mg·ml- 1范围内 ,峰面积与浓度 (mg·ml- 1)呈良好的线性关系 ,r =0 .9998,平均回收率为 99.2 3% ,RSD为 0 .84 % ,日内、日间相对标准偏差均小于 2 % ,精密度较好 ,符合分析测试的要求 ;罗红霉素膜剂热稳定性良好 ,在高湿条件下罗红霉素含量几乎无变化。结论 :罗红霉素膜剂稳定性良好 ,含量测定方法简便 ,专属、重现性好     

HPLC法测定诺氟沙星胶囊含量的改进

目的 :改进诺氟沙星胶囊含量HPLC测定方法。方法 :采用反相高效液相色谱法。色谱柱 :SpherisorbC18柱 ,流动相 :磷酸 -三乙胺缓冲液水乙腈 (6 0 30 10 ) ,流速 :1 0ml·min- 1,检测波长 :2 78nm。结果 :诺氟沙星的浓度在 4 8～ 96 μg·ml- 1范围内线性关系良好 ,回归方程 :A =2 19× 10 4 + 7 4 0×10 4 C(r =0 99998) ,加样回收率平均值为 98 5 %。RSD =0 5 % ,n =5 )。结论 :用本方法测定诺氟沙星胶囊的含量快速、重现性好、专属性强、结果准确可靠     

高效液相色谱法测定盐酸氯胺酮注射液的含量

目的　采用HPLC法测定盐酸氯胺酮注射液的含量。方法　采用AgilentODS色谱柱 ,4 6mm× 2 5 0mm ,5 μm ,流动相 :四氢呋喃 -水 -三乙胺 (5∶95∶0 2 )磷酸调节 pH值 3 5 ,检测波长 :2 6 9nm ,流速为 1 0ml·min-1。结果　加样回收率为99 6 % (RSD为 0 8% ,n =9) ;盐酸氯胺酮在 0 4 0 4mg·ml-1～ 1 6 16mg·ml-1范围内浓度与面积呈良好的线性关系。结论　本法测定盐酸氯胺酮注射液的含量 ,结果准确 ,重复性好     

不同产地胡芦巴中总黄酮和槲皮素的含量测定

目的测定胡芦巴 (Trigonellafoenum graecumL )种子中总黄酮及槲皮素的含量。 方法总黄酮含量测定 :以芦丁为对照品 ,采用分光光度法 ,于 5 10nm处测定 ;槲皮素含量测定 :采用高效液相色谱法 ,色谱柱为KromasilODS— 1,流动相为乙腈 1g·L-1磷酸溶液 (体积比 30∶70 ) ,检测波长 36 0nm。结果总黄酮在 8 4 8～ 5 0 88mg·L-1(r =0 9996 )、槲皮素在 0 18～ 3 6 8mg·L-1(r =0 9995 )内线性关系良好 ;总黄酮和槲皮素的平均回收率分别为 99 4 %、99 3%。结论建立的方法可为胡芦巴的质量控制提供依据     

气相色谱法测定红花籽油中亚油酸的含量

目的　用气相色谱法测定红花籽油中亚油酸的含量。方法　色谱柱为涂布 1 0 %的丁二酸二乙二醇聚酯 (DEGS)固定液的石英玻璃柱 (3mm× 3m) ,柱温 1 80℃ ,检测器温度 2 30℃。结果　亚油酸在 1 5 .0 6～ 90 .44mg·ml- 1 浓度范围内 ,线性关系良好 (A =1 2 6863 .8+1 4 570 0 .4C ,r =0 .9995) ,回收率为 98.75 % ,RSD =1 .2 1 %。结论　该方法可用于红花籽油的质量控制     

HPLC法同时测定毛诃子中5种鞣质类成分的含量

摘要：目的:建立同时测定藏药毛诃子中单宁酸、儿茶素、柯里拉京、诃子鞣酸、鞣花酸5种鞣质类成分的HPLC方法。方法:采用Agilent Zorbax C18色谱柱（250 mm×4.6 mm,5μm）,流动相为乙腈（A）-0.1%磷酸（B）,梯度洗脱;流速:1.0 ml·min-1;检测波长:210 nm;柱温:25℃。结果:毛诃子中5个成分分离度良好,单宁酸、儿茶素、柯里拉京、诃子鞣酸和鞣花酸的质量浓度分别在线性方程分别为0.253 6～2.536 0 mg·ml-1（r=0.999 2）、0.003 5～0.035 0 mg·ml-1（r=0.999 6）、0.007 6～0.076 0 mg·ml-1（r=0.999 3）、0.004 9～0.049 0 mg·ml-1（r=0.999 7）和0.004 4～0.044 0 mg·ml-1（r=0.999 9）范围内与峰面积呈良好的线性关系;精密度、重复性良好,RSD均小于2%;在室温条件下12 h内稳定;平均加样回收率在99.3%～100.3%之间（RSD为1.5%～1.7%,n=9）。结论:该方法简便、准确,重复性好,可用于毛诃子中单宁酸、儿茶素、诃里拉京、诃子鞣酸、鞣花酸5种成分的同时测定。     

HPLC法同时测定复方诺氟沙星滴鼻液中的诺氟沙星和盐酸麻黄碱

目的　建立一种快速、准确的高效液相色谱法同时测定诺氟沙星 ( NOR)和盐酸麻黄碱 ( EPH)的含量。 方法　使用 C1 8色谱柱 ,流动相为乙腈— 0 .1%磷酸 ( 15 :85 V/V) ,检测波长为 2 5 6nm。结果 　样品测定在 9min内完成。诺氟沙星在 10～ 60μg· ml- 1 浓度范围内 ,r=0 .9999,RSD= 0 .46% ,平均回收率为 99.91% ;盐酸麻黄碱在 2 5～ 12 5 μg· ml- 1浓度范围内 ,r=0 .9992 ,RSD=0 .5 1% ,平均回收率为 10 0 .0 3%。 结论 　方法可快速准确地检测复方诺氟沙星滴鼻液中的诺氟沙星和盐酸麻黄碱含量     

HPLC法测定替卡西林钠的含量及有关物质

目的　采用HPLC法测定替卡西林钠的含量及有关物质。方法　色谱柱 :日本岛津液相填充柱C18(2 5 0× 4 6mm5 μm) ;流动相 :磷酸盐缓冲液 (pH4 3) -乙腈 (92∶8) ;UV检测波长 :2 2 0nm。 结果　含量测定在 0 4 1～ 1 19mg·ml-1范围内峰面积与浓度有良好的线性关系 (r =0 9997) ,有关物质测定在 30 84～ 71 96 μg·ml-1范围内峰面积与浓度呈良好的线性关系(r=0 9998)。结论　本方法在测定过程中具有良好的稳定性、专属性及重现性     

高效液相色谱法同时测定滴鼻剂中盐酸麻黄素和氢化可的松的含量

目的 :用HPLC法同时测定滴鼻剂中盐酸麻黄素氢化可的松的含量。方法 :采用C18色谱柱 ,流动相为甲醇 0 .0 5mol·L-1KH2 PO4 三乙胺 (5 0∶5 0∶0 .2 ) ,用磷酸调 pH3.7,检测波长 2 5 7nm。结果 :盐酸麻黄素在 36 0～ 6 0 0 μg·ml-1浓度范围内线性关系良好 (r =0 .9999) ,回收率 10 1.3% ,RSD为 1.0 %。氢化可的松在 36～ 6 0 μg·ml-1浓度范围内线性关系良好 (r =0 .9998) ,回收率 10 1.5 % ,RSD为 1.0 %。结论 :该方法可同时测定滴鼻剂中盐酸麻黄素氢化可的松含量。     

HPLC同时测定银黄含化片中绿原酸和黄芩苷含量

目的　建立HPLC法测定银黄含化片中绿原酸和黄芩苷含量的方法。方法　采用ODS色普柱(25 0mm×4 . 6mm,5 μm),以乙腈- 1%磷酸溶液为流动相进行梯度洗脱,检测波长为316nm。结果　绿原酸、黄芩苷分别在0 . 0 2mg·ml-1～0 . 19mg·ml-1和0 . 1mg·ml-1～0 . 8mg·ml-1浓度范围内呈良好线性关系,平均回收率分别为97. 3%和98. 6 %。结论　方法准确、灵敏,回收率高,可用于该制剂的质量控制     

Eradication of Helicobacter pylori with lansoprazole, roxithromycin and metronidazole—an open pilot study

Background:

The most extensively studied Helicobacter pylori eradication regimen comprises omeprazole, clarithromycin and metronidazole. Macrolide antibiotics other than clarithromycin should achieve similar efficacy, but they have not yet been thoroughly tested.

Aim:

To determine the efficacy and safety of a triple therapy regimen using lansoprazole, roxithromycin, and metronidazole on the basis of multicentre out-patient care in an open pilot study.

Methods:

163 patients with duodenal ulcer and proven H. pylori infection received lansoprazole 30 mg b.d., roxithromycin 300 mg b.d. and metronidazole 500 mg b.d. for 7 days followed by another 7 days of lansoprazole 30 mg once daily. H. pylori status was determined by urease quick test, histology, microbiology and ¹³C-urea breath test before starting and at least 4 weeks after completing treatment.

Results:

150 patients were available for evaluation; H. pylori was successfully eradicated in 84.7% (127/150) as determined by urease quick test, 78.0% (117/150) by histology, 81.3% (109/134) by ¹³C-urea breath test; and in 75.3% (113/150), at least two tests were negative. Side-effects were reported in 34 patients (most commonly diarrhoea and changes in liver function tests), in two cases the study medication was interrupted. Prior to treatment, 23% of the H. pylori isolates were resistant against metronidazole and 3.4% against roxithromycin. After unsuccessful treatment, 84% of the isolates were resistant against metronidazole and 21% against roxithromycin. Primary resistance to metronidazole increased the chance of treatment failure approximately sevenfold (7% vs. 53%).

Conclusions:

For H. pylori eradication, the combination of lansoprazole, roxithromycin and metronidazole proved to be as safe as other current triple therapy regimens, while a comparison of efficacy rates yet remains to be assessed in prospective controlled trials. The metronidazole-resistant H. pylori is not rare in Germany and, in the present study, has strongly influenced treatment success.

     

罗红霉素胶囊溶出度考察

目的:对不同厂家的罗红霉素胶囊进行溶出度比较。方法:采用2000年药典规定的方法测定溶出度,并对其溶出参数(Td、T50、m)进行统计处理。结果:不同厂家之间溶出速率相差很大(P<0.01),B厂最快,C厂最慢。结论:不同厂家的产品内在质量有显著差别。     

罗红霉素胶囊剂的临床药物动力学及相对生物利用度

目的：进行国产与进口罗红霉素的生物利用度研究。方法：通过交叉试验对８名男性志愿者（２２．６ａ±ｓ２．１ａ）交叉口服罗红霉素３００ｍｇ国产胶囊剂和进口片剂,进行单剂量药物动力学研究。血药浓度采用微生物法进行测定。结果：口服国产胶囊和进口片剂的血药浓度＿时间曲线均符合二室模型,Ｃｍａｘ分别为９．５ｍｇ／Ｌ±１．３ｍｇ／Ｌ与９．０ｍｇ／Ｌ±１．０ｍｇ／Ｌ,Ｔｍａｘ为１．１４ｈ±０．１８ｈ与１．３１ｈ±０．２１ｈ,Ｔ１２β为１３．１ｈ±２．４ｈ与１３．６ｈ±２．２ｈ,ＡＵＣ为１０７ｍｇ·ｈ／Ｌ±２３ｍｇ·ｈ／Ｌ与１０８ｍｇ·ｈ／Ｌ±１４ｍｇ·ｈ／Ｌ。比较２种制剂的药物动力学参数,其差别均无显著意义（Ｐ＞０．０５）。与进口罗红霉素片相比较,国产罗红霉素胶囊剂的相对生物利用度为（９８±１３）％。口服该药４８ｈ尿药回收率为给药量的（１５±５）％。结论：国产罗红霉素胶囊体内过程与进口罗红霉素片剂相仿,２种制剂生物等效。     

Characteristic difference in gastrointestinal excretion of clarithromycin and roxithromycin

Excretion characteristics of two new macrolides; clarithromycin and roxithromycin, into the intestinal and the gastric lumens was studied by in situ single-pass perfusion and loop methods in rats. Roxithromycin maintained higher serum levels than clarithromycin after their intravenous administrations at a dose of 5 mg kg⁻¹ each. Radioactivities of clarithromycin and roxithromycin exsorbed into the intestinal lumen were 8.6 and 18.9% of dose in 2 h, respectively, whereas clarithromycin and roxithromycin excreted into the bile were 28.4 and 5.9%, respectively. These results suggest that roxithromycin is transported mainly by exsorption across the intestinal membrane, whereas clarithromycin mainly by excretion through the biliary tract. On the other hand, radioactivities of clarithromycin and roxithromycin exsorbed into the gastric lumen were much less then those into the intestinal lumen and were 0.72 and 1.34% of dose in 4 h, respectively. Thus, the exsorption into the gastric lumen seems to be a minor route for the elimination of both macrolides. Consequently, the transport into the intestinal lumen via the intestinal membrane and/or the bile tract may play a significant role in the overall elimination of both macrolides. © 1998 John Wiley & Sons, Ltd.     

Synthesis of 99mTc‐roxithromycin: A novel diagnostic agent to discriminate between septic and aseptic inflammation

Roxithromycin is a second‐generation macrolide antibiotic derived from erythromycin. In the current study, roxithromycin (ROX) was successfully labeled with technetium‐99m for early diagnosis of bacterial infection and discrimination between septic and aseptic inflammation. The highest radiochemical purity of ≥95% was achieved by investigating different labeling parameters such as pH, ligand/reducing agent concentration, temperature, and amount of stabilizing agent. For this purpose, 0.3–0.5 mg ligand, 2–6 μg SnCl₂·2H₂O as a reducing agent at basic pH (8–10 pH) and 2 mg mannitol used as a stabilizing agent, in the end, 370 MBq ^99mTc added into the reaction vials and incubated for a wide range of temperature (?4 to 65°C). The percent radiochemical purity of ^99mTc‐roxithromycin was assessed with the help of the radio‐thin‐layer chromatography technique. The characterization studies were carried out using electrophoresis and Radio‐HPLC techniques as well as saline stability and serum stability studies were also performed. Furthermore, biodistribution study was also performed in an inflamed animal model to discriminate between septic (heat‐killed Staphylococcus aureus) and aseptic (turpentine oil) inflammatory lesions. The results were elaborated that ^99mTc‐roxithromycin (^99mTc‐ROX) was clearly bounded at the septic inflammation site (T/NT ratio of 7.08 ± 1.14) at 30 min postadministration, and maximum accumulation was seen in heart, lungs, liver, stomach, kidneys, and intestine. The results were suggested that ^99mTc‐ROX might be used to discriminate between septic and aseptic inflammatory lesions at an early stage.     

Decrease in gastrointestinal absorption of roxithromycin in bile duct cannulated rats due to depletion of bile salts

The purpose of this study was to investigate the effect of bile salts on gastrointestinal absorption and the plasma second peak phenomenon of roxithromycin in rats. The pharmacokinetic parameters of roxithromycin were calculated after single oral administration at a dose of 20 mg/kg in sham‐operated (control), bile duct cannulated (BDC) and bile salt co‐administered bile duct cannulated (BSBDC) rats. In BDC rats, the total area under the plasma concentration–time curve from time zero to time infinity (AUC_0–∞) and the peak plasma concentration (C_max) were significantly smaller (0.572‐fold) and lower (0.412‐fold), respectively, than those in the control rats. These values were recovered by co‐administration of bile salt (0.831‐ and 0.828‐fold for AUC_0–∞ and C_max compared with the control, respectively). Thus, the decreased absorption of roxithromycin in BDC rats could be due to a depletion of bile. The solubility of roxithromycin was 3.09‐fold increased at 30 mm of sodium taurocholate. The oral dosage regimen of roxithromycin could be changed in patients with bile deficiency or when the drug is administered to individuals on a high‐fat diet, if the present rat data can be extrapolated to humans. Copyright © 2013 John Wiley & Sons, Ltd.     

HPLC法测定人血清罗红霉素药物浓度

目的建立血清中罗红霉素的高效液相色谱检测法。方法经过二氯甲烷为溶剂的液相提取,采用高效液相色谱法和紫外检测。结果血清中罗红霉素能很好分离,无血浆内源物干扰,最低检测浓度为0.25μg.mL-1,罗红霉素在0.25~24μg.mL-1范围之间线性良好(r=0.999,P<0.01),提取回收率在80%以上,相对回收率在90%附近,日间、日内变异系数均小于10%(n=5)。结论该实验建立的血清中罗红霉素检测法,符合生物样品分析要求。     

RP-HPLC法测定罗红霉素片中罗红霉素的含量

目的建立罗红霉素片含量测定的高效液相色谱法,并与微生物检定法、紫外分光光度法的测定结果进行比较。方法采用Agilent-C18色谱柱（4.6 mm×250 mm,5μm）;0.067 mol·L^-1磷酸二氢铵（三乙胺调节pH6.5）-乙腈（3∶2）,加入1%的三乙胺,用磷酸调节pH7.2为流动相;流速1.0 ml·min^-1;检测波长211 nm;柱温30℃。结果罗红霉素在2.14～42.80 mg·L^-1的浓度范围内有良好的线性关系（r=0.999 9）,平均回收率为97.8%,RSD为0.78%（n=5）。结论三种含量测定方法的结果相近,均可用于罗红霉素片的含量测定。     

罗红霉素缓释胶囊在家犬体内的药动学及相对生物利用度

目的评价罗红霉素缓释胶囊在家犬体内的药动学、相对生物利用度及体内外相关性。方法6条家犬随机交叉口服罗红霉素普通片和罗红霉素缓释胶囊 3 0 0mg后 ,利用HPLC法测定血药浓度并对其进行药动学和生物利用度研究。结果罗红霉素缓释胶囊和普通片的tmax分别为 (6 40±1 67)h和 (1 60± 0 5 5 )h ,cmax分别为 (6 5 2± 1 44)mg·L-1和 (1 5 5 1± 4 3 8)mg·L-1,AUC0 -52 分别为 (1 5 2 99± 3 3 5 2 )mg·h·L-1和 (1 70 86± 446 43 )mg·h·L-1,MRT0 -52 分别为 (2 0 42± 1 1 5 )h和 (1 3 0 3± 2 80 )h ,相对生物利用度为 90 76% ;其体内吸收与体外释药相关性显著 (r =0 9788)。结论罗红霉素缓释胶囊具有明显的缓释特征