HPLC法测定水飞蓟宾胶囊中水飞蓟宾的含量

目的建立高效液相色谱法测定水飞蓟宾胶囊中水飞蓟宾的含量。方法色谱柱：Inertsil ODS-SP（4.6mm×250mm,5μm）;流动相为甲醇-水-冰醋酸（45∶55∶1.0）,检测波长为287nm,流速为1mL.min-1。结果水飞蓟宾对照品在10.13μg.mL-1~101.30μg.mL-1浓度范围内与峰面积呈良好线性关系（r=0.9998）,平均回收率99.72%,RSD%=0.55%（n=9）。结论本方法操作简便、准确、重复性好,可作为该制剂的定量分析方法。     

HPLC法测定贝那普利氢氯噻嗪片的有关物质

目的建立高效液相色谱法测定贝那普利氢氯噻嗪片的有关物质。方法采用Ultimate AQ-C18色谱柱(250mm×4.60mm,5μm);流动相:四氢呋喃-水-冰醋酸(250mL+750mL+4mL,加入四丁基溴化铵1.0g);流速:1.5mL·min-1;检测波长:240和316nm。结果杂质CGS14831的线性范围为3.74~28.08μg·mL-1,相关系数r=0.999 6;杂质CGP42454A、CGS 14829A的线性范围为1.63~12.19μg·mL-1:相关系数r=0.999 5;杂质SU5683的线性范围为2.03~15.24μg·mL-1,相关系数r=0.999 7。结论该方法重复性好,结果准确,能更好地控制贝那普利氢氯噻嗪片中有关物质的含量。     

HPLC法同时测定氨麻苯美片中4种主要成分的含量

目的:建立同时测定氨麻苯美片中盐酸伪麻黄碱、对乙酰氨基酚、氢溴酸右美沙芬和盐酸苯海拉明等成分含量的HPLC方法。方法:色谱柱为Kromasil 60-5CN(25 mm×4.6 mm,5μm)柱;以乙腈-pH3.0的40 mmol.L-1三乙胺水溶液(20∶80)为流动相;检测波长为215 nm;流速为1.0 mL.min-1。结果:盐酸伪麻黄碱、对乙酰氨基酚、氢溴酸右美沙芬和盐酸苯海拉明的线性范围分别为6.036~150.9μg.mL-1(r=1.0000),65.42~1636μg.mL-1(r=0.9989),3.010~75.25μg.mL-1(r=1.0000),50.90~127.2μg.mL-1(r=1.0000);加样回收率(n=9)分别为98.5%,100.9%,99.1%和99.6%。结论:本法简单、快速、准确,可用于氨麻苯美片中4种主要成分的同时测定。     

HPLC法测定头孢羟氨苄甲氧苄啶胶囊含量的方法改进

目的建立调整流动相比例,以HPLC法同时测定复方头孢羟氨苄甲氧苄啶胶囊中头孢羟氨苄与甲氧苄啶的含量的方法。方法色谱柱SinoChrom ODS-BP C18柱(4.6mm×250mm,5μm);流动相:1%冰醋酸(含0.005%乙二胺)溶液∶乙腈(88∶12);流速:1.0mL.min-1;检测波长:233nm。结果头孢羟氨苄在40.00~200μg.mL-1浓度范围之间线性良好,r=0.9999,平均回收率为99.8%,RSD%=0.33%(n=5);甲氧苄啶在8~40μg.mL-1浓度范围之间线性良好,r=1.000,平均回收率为100.1%,RSD%=0.28%(n=5);。结论以本文中采用的流动相,头孢羟氨苄主峰与溶剂峰、头孢羟氨苄峰与甲氧苄啶峰分离完全,结果准确稳定,可用于头孢羟氨苄甲氧苄啶胶囊的含量测定。     

凝胶色谱法测定头孢克洛胶囊聚合物的含量

目的建立凝胶色谱法(SEC)测定头孢克洛胶囊聚合物.方法采用依利特色谱柱(填料:Sephadex G-10;尺寸:10.0mm×300mm);流动相A为pH 7.0的0.05mol?L-1的磷酸盐缓冲液[0.05mol?L-1的磷酸氢二钠溶液-0.05mol?L-1的磷酸二氢钠溶液(61∶39)],流动相B为超纯水;流速1.0mL?min-1;检测波长为254nm;进样量为100μL;以头孢噻肟对照品为替代对照品进行测定,按外标法定量.结果 头孢噻肟的线性范围为1.03μg?mL-1～10.29μg?mL-1(r=0.9999),定量限为1×10-3mg?mL-1,重复性良好(RSD为0.44%,n=5);供试品测定的线性范围为11mg?mL-1～46mg?mL-1(r=0.9997),重复性良好(RSD为2.76%,n=5).结论 该方法能够较好地分离头孢克洛和聚合物,可用于头孢克洛胶囊聚合物的检验.     

气相色谱法测定非布索坦中残留有机溶剂的含量

目的建立非布索坦中4种有机溶剂残留量的分离测定方法。方法采用溶液直接进样气相色谱法,色谱柱为PEG-20M填充柱(2 m×3 mm),载气为氮气,以二甲基亚砜为溶剂,测定了非布索坦原料药中丙酮、乙酸乙酯、乙醇与N,N-二甲基甲酰胺的残留量。结果 4种有机溶剂完全分离,在所考察的浓度范围内线性关系良好,其中丙酮的线性范围在1.056~105.6μg.mL-1(r=0.999 8),乙酸乙酯的线性范围在1.028~102.8μg.mL-1(r=0.999 98),乙醇的线性范围在0.992~99.2μg.mL-1(r=0.999 8),N,N-二甲基甲酰胺的线性范围在0.361~36.1μg.mL-1(r=0.999 8)。各残留溶剂的精密度试验RSD均小于5%,平均回收率在97.75%~102.83%之间。结论本实验所建立的方法简便、灵敏、准确,可用于非布索坦中有机溶剂残留量的测定。     

HPLC梯度洗脱法测定丙泊酚中/长链脂肪乳注射液的含量及有关物质

目的：建立测定丙泊酚中/长链脂肪乳注射液中的丙泊酚及其有关物质的HPLC方法。方法：色谱柱为Waters XBridge RP18柱（4.6mm×150mm,5μm）;流动相为磷酸二氢钠溶液-乙腈,梯度洗脱;柱温为40℃;检测波长为275nm和254nm。丙泊酚的测定采用外标法,有关物质检查采用外标法与自身对照法。结果：丙泊酚与其两杂质能较好分离,相邻各峰间分离度均大于1.5;丙泊酚、杂质Ⅰ和杂质Ⅱ的线性范围分别为97.2~1457.9μg?mL-1（r=0.999 9）、0.11～1.57μg?mL-1（r=0.999 9）和0.11～1.59μg?mL-1（r=0.999 9）;平均回收率（n=9）分别为99.2%（RSD＝1.4%）、105.8%（RSD＝1.5%）和96.7%（RSD＝4.8%）。结论：所建方法简便快速、专属性强、重复性好,可用于丙泊酚中/长链脂肪乳注射液的含量测定和杂质检查。     

HPLC法测定八维钙锌片中维生素D_2和维生素E的含量

目的:建立RP-HPLC法测定八维钙锌片中维生素D2和维生素E含量的方法。方法:采用Phenomenex-C18柱(4.6 mm×150 mm,5μm);以为甲醇流动相;紫外检测波长为265 nm;流速为1 mL.min-1。结果:维生素D2的线性范围为0.8473～4.2365μg.mL-1(r=0.9996),平均回收率为99.7%,RSD%为1.82%(n=9);维生素E的线性范围为0.1625～0.8125mg.mL-1(r=0.9996),平均回收率为100.3%,RSD%为1.93%(n=9)。结论:本方法操作简便,结果准确、可靠,可同时测定八维钙锌片中维生素D2和维生素E的含量。     

UPLC快速测定葛根芩连汤肠外翻囊样品中6个黄酮类成分含量

目的:建立UPLC法同时测定葛根芩连汤肠外翻囊样品中6个黄酮类成分(葛根素、大豆苷、甘草苷、野黄芩苷、黄芩苷、汉黄芩苷)的含量。方法:样品用甲醇提取,采用Agilent Proshell 120 EC-C18(4.6 mm×50 mm,2.7μm)色谱柱,以0.2%醋酸水溶液(A)-甲醇(B)为流动相进行梯度洗脱,流速1 mL.min-1,紫外检测波长270 nm,柱温30℃。结果:葛根素、大豆苷、甘草苷、野黄芩苷、黄芩苷、汉黄芩苷质量浓度分别在0.1870～93.50μg.mL-1(r=0.9999),0.02730～13.65μg.mL-1(r=0.9999),0.02550～12.75μg.mL-1(r=0.9999),0.05580～27.90μg.mL-1(r=0.9998),0.2124～106.2μg.mL-1(r=0.9999),0.09140～45.70μg.mL-1(r=0.9999)范围内有良好的线性关系;日间、日内精密度变异均小于2%;平均回收率(n=9)分别为101.4%,97.88%,99.15%,99.72%,98.50%,101.4%;稳定性良好。结论:所建立的分析方法操作简便、快速、灵敏,结果准确,重复性好,所需样品少,并已成功应用于葛根芩连汤大鼠肠吸收动力学的研究。     

五维B颗粒质量标准的研究

目的建立检测五维B颗粒的质量标准。方法采用高效液相色谱法来对五维B颗粒中的烟酰胺、维生素B1、维生素B2、维生素B6进行定性和定量分析,ODS柱（250mm×4.6mm,5μm）,流动相：甲醇-5mmol﹒ml^-1庚烷磺酸钠（含0.5%冰醋酸＋0.1%三乙胺）（28：72）,检测波长为280nm,流速1.0ml﹒min^-1。结果烟酰胺、维生素B1、维生素B2、维生素B6的线性回归方程为：A烟酰胺=241702C＋255124,r=1.0000,n=3;A维生素B1=191550C-1691.3,r=1.0000,n=3;A维生素B2=266250C-3098.3,r=1.0000,n=3;A维生素B6=14448C＋139.4,r=1.0000,n=3;线性范围分别为：105.25～631.50μg﹒ml^-140.05～240.30μg﹒ml^-121.35～128.10μg﹒ml^-14.15～24.90μg﹒ml^-1结论该方法准确,灵敏度高,重现性好,可作为质量检验的定量方法。     

Fondaparinux Sodium Compared with Enoxaparin Sodium

INTRODUCTION: Patients undergoing major orthopedic surgery face considerable risk of venous thromboembolism (VTE), which may be fatal unless they receive prophylactic treatment. Fondaparinux sodium is a new antithrombotic agent that is indicated for prophylaxis of VTE after major orthopedic surgery. This paper presents a cost-effectiveness analysis of fondaparinux sodium and enoxaparin sodium, the latter being the most commonly used agent for prophylaxis of VTE. METHODS: The analysis is based on an international simulation model, using Norwegian unit costs, and Norwegian data of 55 000 patients undergoing orthopedic surgery between 1999 and 2001. We estimated the expected incidence of VTE and VTE-related deaths, and expected costs of VTE-related care for each of the two prophylactic agents for different periods. RESULTS AND CONCLUSION: The results indicate that fondaparinux sodium is likely to be more effective than enoxaparin sodium in preventing the incidence of VTE. By day 90, fondaparinux sodium is expected to avoid 180 more VTE events, and between 8 and 33 more VTE-related deaths per 10,000 patients than enoxaparin sodium. Fondaparinux sodium is also a cost-saving option in short follow-up periods for hip fracture surgery. For extended follow-up periods (i.e. 5 years), fondaparinux sodium is also likely to represent the lower cost treatment option after total knee and hip replacement. The sensitivity analyses show that the main results are robust to changes in the most important parameters. Results are, however, sensitive to the price difference between the two drugs.     

国家食品药品监督管理局国家药品标准修订——注射用阿莫西林钠氟氯西林钠

本品为阿莫西林钠与氟氯西林钠[阿莫西林(C₁₆H₁₉N₃O₅S)与氟氯西林(C₁₉H₁₇ClFN₃O₅S)标示量之比为1:1]均匀混合制成的无菌粉末。按无水物计算,每1 mg含阿莫西林(C₁₆H₁₉N₃O₅S)和氟氯西林(C₁₉H₁₇ClFN₃O₅S)分别不得少于400 μg和436 μg。按平均装量计算,含阿莫西林(C₁₆H₁₉N₃O₅S)和氟氯西林(C₁₉H₁₇ClFN₃O₅S)均应为标示量的90.0%~110.0%。     

注射用他唑巴坦钠/哌拉西林钠

本品为哌拉西林钠和他唑巴坦钠组成的复方制剂。哌拉西林为广谱半合成着霉素类抗生素，他唑巴坦为β-内酰胺酶抑制剂。本品适用于对哌拉西林耐药，但对哌拉西林／他唑巴坦敏感的产β-内酰胺酶的细菌引起的中、重度感染，其抗菌谱包括革兰氏阴性菌、革兰氏阳性菌及厌氧菌。     

国家食品药品监督管理局国家药品标准修订件——注射用阿莫西林钠舒巴坦钠

本品为白色或类白色粉末或结晶性粉末,极易引湿。     

HPLC法测定头孢哌酮钠/舒巴坦钠中头孢哌酮钠的胆药浓度

目的:建立头孢哌酮钠/舒巴坦钠中头孢哌酮钠胆药浓度的测定方法。方法:于腹腔镜胆囊切除手术中胆囊取胆汁标本,用高效液相色谱法测定胆清中头孢哌酮钠的浓度,其中色谱柱为YWGC18,流动相为甲醇-水-冰醋酸(25.5∶74.5∶0.45),流速为1.0mL.min-1,柱温为35℃,检测波长为254nm。结果:头孢哌酮胆汁浓度在1.25~62.5μg.mL-1范围内线性关系良好(r=0.9991);平均回收率为95.14%(RSD=3.42%)。结论:本方法简便、可靠,可为临床合理用药提供依据。     

国家食品药品监督管理局国家药品标准修订——萘夫西林钠

本品为(2S,5R,6R)-6-(2-乙氧基-1-萘甲酰胺基)-3,3-二甲基-7-氧-4-硫杂-1-氮杂双环[3.2.0]庚烷-2-甲酸-钠-水合物。按无水物计算,含萘夫西林(C₂₁H₂₂N₂O₅S)不得少于85.5%。     

Fondaparinux Sodium

Fondaparinux sodium (fondaparinux) is a synthetic sulfated pentasaccharide anticoagulant developed from the antithrombin binding moiety of heparin. Through the activation of antithrombin it inhibits Factor Xa, the activation of thrombin, and the subsequent coagulation cascade. Fondaparinux is approved in Europe and the US for the treatment of acute venous thromboembolism (VTE), including both deep vein thrombosis (DVT) and pulmonary embolism (PE), when used in conjunction with warfarin. In phase III clinical trials, subcutaneous fondaparinux was noninferior to subcutaneous enoxaparin or intravenous unfractionated heparin (UFH) in the prevention of recurrent symptomatic VTE in patients with acute DVT and PE, respectively, and equally well tolerated. It thus provides a valuable alternative to UFH and low-molecular weight heparins in the treatment of acute VTE, particularly in the outpatient setting.     

Fondaparinux Sodium

Fondaparinux sodium (Arixtra) is a synthetic, sulfated pentasaccharide, selective factor Xa inhibitor that is indicated in Europe for preventing thrombus formation in patients with acute coronary syndromes (ACS; the focus of this review), including those with ST-segment elevation myocardial infarction (STEMI), non-STEMI (NSTEMI), or unstable angina.The large (n = 20,078), well designed OASIS-5 trial showed that subcutaneous fondaparinux 2.5 mg/day for 12,000) OASIS-6 trial. There were no differences in the incidence of major bleeding between these groups, resulting in a benefit : risk balance favoring fondaparinux. The specificity and selectivity of fondaparinux, combined with its long half-life and 100% bioavailability, allows once-daily anticoagulation without the need for monitoring activated clotting time. Subcutaneous fondaparinux was noninferior to enoxaparin treatment in patients with unstable angina or NSTEMI, and was more effective than usual care in those with STEMI. Fondaparinux has a favorable tolerability profile, particularly with regard to the risk of major bleeding, and limited data suggest that it is more cost effective than enoxaparin in the short term. Thus, overall, clinical evidence suggests that fondaparinux has a valuable place in the treatment of patients with ACS.     

国家食品药品监督管理局国家药品标准修订件——甘氨双唑钠

本品为类白色至微黄色的结晶或结晶性粉末;无臭,味苦;遇光色渐变深。