HPLC法同时测定盐酸平阳霉素和地塞米松磷酸钠的含量

目的:建立同时测定盐酸平阳霉素和地塞米松磷酸钠含量的方法。方法:采用高效液相色谱法。色谱柱为依利特Hypersil ODS2 C18,流动相为乙腈-水(28∶72,V/V),流速为1.0 ml/min,检测波长为250 nm,柱温为30.0℃,进样量为20μl。结果:盐酸平阳霉素和地塞米松磷酸钠的检测质量浓度分别在0.03².10、0.022.10、0.02¹.10 mg/ml范围内与各自峰面积积分值呈良好的线性关系(r=0.999 9、r=0.999 7);精密度、稳定性、重复性试验的RSD≤0.88%;平均加样回收率分别为100.05%、99.81%,RSD分别为0.77%、1.33%(n=9)。结论:该方法简便、快速、准确、灵敏度高,可用于同时测定盐酸平阳霉素和地塞米松磷酸钠的含量。     

高效液相色谱法测定青霉素V钾片中主药的含量

目的:建立以高效液相色谱法测定青霉素V钾片中主药含量的方法。方法:色谱柱为DiamonsilC18,流动相为乙腈-0.02mol/L醋酸钠(70∶30),流速为1.0ml/min,检测波长为268nm,灵敏度为0.01AUFS,柱温为(26±1)℃,进样量为20μl。结果:青霉素V钾检测浓度在10.0～120.0μg/ml范围内与峰面积呈良好的线性关系(r=0.9999,n=5);平均加样回收率为100.2%(RSD=0.42%)。结论:本方法快速、简便、准确,可用于青霉素V钾片的质量控制。     

高效液相色谱法测定利福霉素钠含量与有关物质

目的建立高效液相色谱法测定注射用利福霉素钠含量及其有关物质的方法。方法色谱柱AlltechAlltimaC18(250mm×4.6mm,5μm);柱温35℃;流动相甲醇∶乙腈∶0.075mol/L磷酸二氢钾溶液∶1.0mol/L柠檬酸溶液(33∶33∶31∶4);流速1.0ml/min;检测波长254nm;进样量10μl。结果利福霉素的线性范围为0.01mg/ml～4.50mg/ml,r=1.0000,日内RSD为0.2%,日间RSD为0.1%～0.2%,平均回收率为99.7%(n=9),最低检测限为5.4ng。结论本方法简便快速,专属性好,精密度高,准确可靠,可作为控制利福霉素钠与注射用利福霉素钠含量及其有关物质质量的分析方法。     

高效液相色谱法同时测定氯地滴耳液中主药的含量

目的 :建立测定氯地滴耳液中氯霉素和地塞米松磷酸钠含量的高效液相色谱法。方法 :色谱柱为KromasilC8 柱 ,流动相为甲醇 -0 34 %磷酸二氢钾水溶液 (60∶40 ,V/V) ,检测波长为240nm。结果 :氯霉素在100～500μg/ml范围内浓度与峰面积线性关系良好 ,r=0 9999 ,回收率为98 5 %～100 8 % ,RSD≤1 5 % ;地塞米松磷酸钠在16～80μg/ml范围内浓度与峰面积线性关系良好 ,r=0 9990 ,回收率为98 8 %～100 6 % ,RSD≤2 0 %。结论 :该方法可用于同时测定氯地滴耳液中氯霉素和地塞米松磷酸钠的含量。     

HPLC法测定6-氨基青霉烷酸中苯乙酸和青霉素G含量

目的 建立6-氨基青霉烷酸中苯乙酸和青霉素G含量的测定方法.方法 用苯基柱;甲醇pH3.5磷酸盐缓冲溶液水(301060)为流动相;检测波长220nm;流速1.5ml/min;进样量10μl.结果 6-氨基青霉烷酸、苯乙酸峰和青霉素G峰完全分离;样品连续测定6次,苯乙酸和青霉素G的RSD分别为0.89%和0.92%;苯乙酸在0.005～0.040 mg/ml范围内、青霉素G在0.011～0.086 mg/ml 范围内呈良好的线性关系(相关系数均大于0.9999);苯乙酸和青霉素G平均回收率分别为99.12%(RSD=2.8%)和100.05%(RSD=1.O%);检测限分别为3.36×10-5和4.61×10-5mg/ml;定量限分别为1.135×10-4和1.076×10-5mg/ml.结论 该方法专属性好、准确度高,可用于6-氨基青霉烷酸中杂质苯乙酸和青霉素G的含量测定.     

HPLC法同时测定加替沙星和奥硝唑的含量

目的建立同时测定加替沙星及奥硝唑含量的高效液相色谱方法。方法分析柱为Hy-persil-ODSC18柱(250mm×4.6mm,5μm);流动相为0.02mol/L磷酸二氢钾缓冲液(含0.5%三乙胺,用磷酸调pH3.0):甲醇:乙腈(65:18:17);流速:1ml/min;加替沙星、奥硝唑检测波长分别为292nm、318nm;柱温为30℃,进样量20μl。结果加替沙星线性浓度范围为8.0～48.0μg/ml(r=0.9998),日内RSD≤0.52%,日间RSD≤0.92%,平均回收率100.53%;奥硝唑线性浓度范围为8.0～48.0μg/ml(r=0.9999),日内RSD≤0.35%,日间RSD≤0.71%,平均回收率100.56%。结论该方法简便、准确、灵敏,可用于同时测定加替沙星和奥硝唑两组分的含量。     

HPLC测定皮湿霜中苯佐卡因、地塞米松磷酸钠和醋酸氯己定含量

目的:建立 HPLC 测定皮湿霜中苯佐卡因、地塞米松磷酸钠和醋酸氯己定含量的方法。方法:色谱柱:YWG C_(18)分析色谱柱(4.6mm×250 mm,10μm);流动相:甲醇-水(62:37,含0.3%三乙胺,磷酸调 pH 3.0);流速1 mL·min~(-1);检测波长240 nm。结果:苯佐卡因、地塞米松磷酸钠和醋酸氯己定的理论板数分别为5600,3500,3200;回归方程分别为:Y=1.382×10~7+1.550×10~7X(r=0.9998),Y=6.563×10~4+3.220×10~7X(r=0.9995),Y=-2.032×10~6+6.168×10~7X(r=0.9999);线性范围分别为6～18,0.09～0.27,0.6～1.8μg;平均回收率分别为97.6%(RSD=2.3%),96.8%(RSD=3.3%),102.4%(RSD=2.1%)。结论:本法操作简便,结果准确可靠,可用于皮湿霜中苯佐卡因、地塞米松磷酸钠和醋酸氯己定的含量测定。     

注射用氨苄西林钠舒巴坦钠含量测定方法的改进

目的:改进注射用氨苄西林钠舒巴坦钠含量测定方法。方法:ODS柱(150×6.0mm,5μm),流动相:含0.005mol/L氢氧化四丁基铵和0.02mol/L醋酸铵的溶液—乙腈(825:175),用冰醋酸调节pH值为5.0。结果:氨苄西林和舒巴坦的线性范围和回归方程分别为:62～1232μg/ml,C=0.31546A—10.507(r=0.9999);31～621μg/ml,C=0.75961A—2.342(r=1.0000)。本方法与药典方法的测定结果一致。结论:本方法简便、准确、耐用性好。     

高效液相色谱法测定牛奶中的青霉素G和苯唑青霉素

用离子对高效液相色谱法测定牛奶中青霉素G和苯唑青霉素,牛奶试样经丙酮脱蛋白,二氯甲烷抽提,然后在μ-Bondapak C_18柱上进行色谱分离测定。流动相为EDTA(0.005mo1/L):CH_3OH(47:53)1000ml溶液中加入四丁基氯化胺4ml。采用紫外检测器测定这两种青霉素。方法简便、灵敏、准确。青霉素G和苯唑青霉素的回收率分别为89.0～92.5％和89.0～93.6％。测定的相对偏差分别为6.77％和3.49％。检测极限分别为27.3ng/ml和11.5ng/ml。     

高效液相色谱法测定复方达克罗宁乳膏中盐酸达克罗宁、马来酸氯苯那敏、地塞米松磷酸钠的含量

目的建立高效液相色谱法测定复方达克罗宁乳膏中盐酸达克罗宁、马来酸氯苯那敏、地塞米松磷酸钠含量的方法。方法采用高效液相色谱法。色谱柱为VP-ODS C18柱(250 mm×4.6 mm,5μm);流动相为磷酸缓冲液-乙腈(80∶20);流速:1.0 mL.min-1;测定波长:240 nm;柱温:30℃:进样:10μL。结果该方法不受处方中基质干扰。盐酸达克罗宁、马来酸氯苯那敏、地塞米松磷酸钠的线性范围分别为0.100 3~0.702 1μg(r=0.999 8,n=6),0.028 56~0.199 9μg(r=0.999 9,n=6),0.006 694~0.046 85μg(r=0.999 7,n=6),平均回收率分别为98.8%、99.0%、99.0%,RSD分别为0.97%、1.3%、0.98%(n=9)。结论该方法操作简便,灵敏度高,重现性好,可用于复方达克罗宁乳膏中盐酸达克罗宁、马来酸氯苯那敏、地塞米松磷酸钠的含量测定。     

高效液相色谱法测定膦甲酸钠氯化钠注射液中膦甲酸钠的含量

目的建立HPLC法测定膦甲酸钠氯化钠注射液中膦甲酸钠含量的方法.方法采用阴离子交换柱(Waters IC Pak A柱,50 mm× 4.6 mm,5 μm);以0.05 mol·L-1邻苯二甲酸氢钾溶液(取邻苯二甲酸氢钾0.204 g,加水适量,振摇使溶解,加1mol·L-1硝酸溶液5 mL,加水稀释至2 000 mL,摇匀即得)为流动相;流速1.4 mL·min-1,检测波长290nm.结果本方法在0.98～4.90g·L-1浓度范围呈良好线性关系(r=0.999 4),进样重现性RSD为0.71%(n=5),平均回收率为98.93%.结论本法简便、快速、结果准确可靠,可用于膦甲酸钠氯化钠注射液中膦甲酸钠的含量测定.     

Talaporfin sodium

Importance of the field: Despite therapeutic advances, cancer remains the cause of an estimated 23% of deaths in the USA. New treatments for malignancy are greatly needed.

Areas covered in this review: Talaporfin sodium is a light-activated drug that causes tissue death through induction of apoptosis. Systemic antitumor effects mediated by CD8⁺ T cells have been demonstrated in preclinical studies, providing a mechanism for distant response of tumors noted in clinical trials. Talaporfin sodium is approved in Japan for early-stage endobronchial cancer. Phase I and II studies in solid tumors have shown tumor regression in patients refractory to other therapies. Phase III pivotal studies against hepatocellular carcinoma as monotherapy and liver-metastatic colorectal cancer in combination with chemotherapy are ongoing. Talaporfin sodium is also in studies in men with symptomatic benign prostatic hyperplasia. Substantial safety data from clinical trials so far indicate that the drug is well tolerated.

What the reader will gain: Talaporfin sodium has a broad safety profile and a mode of action that could affect growth in treated and untreated tumors.

Take home message: Clinical and preclinical studies indicate that talaporfin sodium treatment may offer a powerful option to synergize current therapies, as well as an alternative monotherapy in treating cancer.     

头孢哌酮钠-舒巴坦钠致血小板减少

1名83岁男性患者因胆道系统感染,静脉给予注射用头孢哌酮钠-舒巴坦钠2.0g,1次/白天;1.0g,1次/晚上。用药6d内血小板进行性下降,由164×109/L下降到68×109/L。停用头孢哌酮钠-舒巴坦钠,改用左氧氟沙星治疗。1周后患者PLT恢复正常。     

哌拉西林钠他唑巴坦钠致抽搐

1例26岁男性患者,4年前行肾移植术,近5个月接受血液透析,因肺部感染给予哌拉西林钠他唑巴坦钠4.5 g加入0.9%氯化钠注射液100 ml、1次/d静脉滴注。第2次用药后5 h,患者突发抽搐、意识丧失、双眼上翻、双腿抽动。先后给予地西泮10 mg肌内注射及7 mg静脉注射,上述症状消失。     

Dalteparin sodium

Dalteparin sodium (Fragmin?, Pharmacia Corporation) is a low molecular weight heparin (LMWH) with a mean molecular weight of approximately 5000 Da. As with the other LMWHs, dalteparin sodium has certain advantages over unfractionated heparin (UFH), most important of which are improved bio-availability by sc. injection, a prolonged antithrombotic activity which is highly correlated with body weight permitting the o.d. administration of the drug. Dalteparin sodium has been subjected to a large number of well-designed randomised clinical trials for the prevention and treatment of thrombotic disorders. Based on data from the randomised clinical trials, dalteparin sodium has been approved internationally for a wide spectrum of clinical indications (e.g., prevention of thromboembolic events after surgery). Dalteparin sodium has also been studied in randomised controlled trials in the maintenance of graft patentcy following peripheral vascular surgery, in place of warfarin for the long-term treatment of patients presenting with deep vein thrombosis (DVT), in the prevention of upper extremity thrombosis in patients with indwelling portacath devices and in pregnant patients with a history of previous venous thromboembolism with or without thrombophilia. Dalteparin sodium has been compared with heparin for the prevention of thrombotic complications during haemodyalisis and haemofiltration. These studies have shown promising results but further work is required before dalteparin sodium can be recommended for these indications.     

Inhaled sodium metabisulphite induced bronchoconstriction: inhibition by nedocromil sodium and sodium cromoglycate.

1. The effects of nedocromil sodium and sodium cromoglycate on bronchoconstriction induced by inhaled sodium metabisulphite have been studied in eight atopic subjects, three of whom had mild asthma. 2. Nedocromil sodium (4 mg, 7.8 X 10(-6) M), sodium cromoglycate (10 mg, 24.1 X 10(-6) M) and matched placebo were administered by identical metered dose inhalers 30 min before a dose-response to sodium metabisulphite (5-100 mg ml-1) was performed. 3. Maximum fall in sGaw after placebo pre-treatment was -43.9 +/- 3.3% baseline (mean +/- s.e. mean). At the same metabisulphite concentration maximum fall in sGaw after sodium cromoglycate was -13.0 +/- 3.6% and after nedocromil sodium was +4.3 +/- 6.8%. Nedocromil sodium prevented any significant fall in sGaw even after higher concentrations of metabisulphite. 4. Both nedocromil sodium, 4 mg, and sodium cromoglycate, 10 mg, inhibited sodium metabisulphite induced bronchoconstriction but nedocromil sodium was significantly more effective. Relative in vivo potency of the two drugs is broadly in line with other in vivo and in vitro studies.     

Fondaparinux sodium

black triangle Fondaparinux sodium, a selective factor Xa inhibitor, is the first in a new class of antithrombotics. It binds selectively with high affinity to antithrombin III and specifically catalyses the inactivation of factor Xa. The elimination half-life of fondaparinux sodium permits once daily treatment. black triangle A randomised, double-blind, parallel-group, dose-ranging, multicentre phase IIb study in 933 eligible patients established that a subcutaneous dose of between 1.5 and 3mg of fondaparinux sodium has the optimum efficacy and safety profile for prophylaxis of venous thromboembolism in patients undergoing major orthopaedic surgery. black triangle Fondaparinux sodium, given to more than 3600 patients undergoing major orthopaedic surgery who participated in prospective, randomised, double-blind, multicentre phase III clinical trials, significantly reduced the incidence of venous thromboembolism, with an overall risk reduction of 55.2% compared with enoxaparin. black triangle Fondaparinux sodium was well tolerated by patients undergoing major orthopaedic surgery, and at the recommended clinical dose of 2.5mg has a similar tolerability profile, including bleeding events, to standard enoxaparin regimens. Fondaparinux sodium has not been reported to cause antibody-induced thrombocytopenia.     

哌拉西林钠他唑巴坦钠致白细胞减少

1例46岁女性患者,因术后颅内感染静脉滴注哌拉西林钠他唑巴坦钠4.5 g,1次/8 h。用药第13、15天外周血白细胞计数从用药前的10.61×109/L分别降至1.79×109/L和1.00×109/L。立即换用其他抗菌药物,同时给予重组人粒细胞巨噬细胞集落刺激因子(rhGM-CSF)150μg皮下注射,1次/d。改变治疗后4 d,血白细胞计数升至6.95×109/L。改变治疗后6 d脑脊液白细胞数由首次用药后15 d的8×106/L升至56×106/L,再次给予哌拉西林钠他唑巴坦钠4.5 g静脉滴注,1次/8 h,rhGM-CSF剂量未变。用药6 d颅内感染治愈,遂停用抗菌药物。治疗第2、5天白细胞计数分别为2.67×109/L和1.65×109/L。第8天停用rhGM-CSF后为5.75×109/L,第15天为4.56×109/L。     

Danaparoid sodium

Danaparoid sodium (Orgaran?, Organon) is a heparinoid glycosaminoglycuronan antithrombotic agent approved for the prophylaxis of post-operative deep vein thrombosis (DVT), which may lead to pulmonary embolism (PE) in patients undergoing elective hip replacement surgery. Danaparoid is a low molecular weight heparinoid consisting of a mixture of heparan sulphate (84%), dermatan sulphate (12%) and small amounts of chondroitin sulphate (4%), whose antithrombotic activity has been well established. Its pharmacological effect is exerted primarily by inhibiting Factors Xa (FXa) and IIa (FIIa) at a ratio greater than heparin, with a minimal effect on platelet function. Danaparoid exhibits low cross-reactivity with heparin-induced antibodies when compared with heparin or low molecular weight heparins (LMWH), thereby making it an excellent choice for the management of heparin-induced thrombocytopenia (HIT). It has excellent bioavailability following sc. injection. Danaparoid has little effect on routine coagulation tests (activated partial thromboplastin time [aPTT], prothrombin time [PT], and thrombin time [TT]). Patients with elevated serum creatinine should be monitored carefully. For its FDA approved indication (DVT prophylaxis during hip replacement surgery), its cost per day is approximately eight times more than LMWH. Even though monitoring is not routinely necessary according to the manufacturer for its approved indication, monitoring is frequently necessary when it is used in other clinical scenarios. Its higher cost than comparable therapies for DVT prophylaxis and the low availability of the FXa assay in most non-tertiary care hospitals has limited the widespread use of danaparoid. Danaparoid has been found to be effective in the treatment of HIT although this is an off label use, despite being the most frequent reason why danaparoid is used.