HPLC法同时测定头孢拉定和精氨酸的含量

以ＨＰＬＣ外标法同时测定注射用头孢拉定（含精氨酸）中头孢拉定、精氨酸和杂质头孢氨苄的含量。方法;采用ＳｐｈｅｒｉｓｏｒｂＣ１８柱,乙腈－醋酸盐缓冲液（１２：８８）为流动相,检测波长２００ｎｍ。结果：该法能罗好地分离被测组分和有关杂质,被测组分的线性关系良好,回收率满意,结论：该法专属性好,快速,准确。     

头孢拉定原料及制剂的聚合物杂质分析#br#

目的 建立头孢拉定原料及制剂中聚合物杂质的分析方法。方法 采用碱降解法制备头孢拉定强制降解溶液;采用高效凝胶色谱法(TSK G2000 SWxl)和柱切换-LC/MS法对头孢拉定强制降解溶液中的聚合物杂质进行分离和结构鉴定;采用Agilent ZORBAX SB-C18型色谱柱,以磷酸盐缓冲液-甲醇为流动相,进行梯度洗脱,建立头孢拉定聚合物的RP-HPLC分析方法,采用二维液相色谱法和柱切换-LC/MSn法对该方法的专属性进行分析;进行方法学验证。结果 在头孢拉定强制降解物中鉴定出头孢拉定二聚体、三聚体、四聚体;高效凝胶色谱法分离头孢拉定聚合物杂质时,易受到小分子杂质的干扰,同时分离的聚合物杂质色谱峰拖尾严重,存在肩峰,定量准确性差;RP-HPLC法分析头孢拉定聚合物杂质时,在20~22min范围内检出头孢拉定二聚体、三聚体、四聚体;方法定量限为500μg,最低检测限为150μg。结论 高效凝胶色谱法不能对头孢拉定中的聚合物杂质进行有效质控,建立的反相色谱法分析头孢拉定聚合物杂质时专属性良好、灵敏度高、方法耐用性好,可用于头孢拉定原料及制剂的聚合物杂质质控;头孢拉定强制降解溶液可作为头孢拉定聚合物分析的系统适用性溶液。     

HPLC法测定盐酸川芎嗪的含量

目的采用高效液相色谱法(HPLC)对盐酸川芎嗪葡萄糖注射液中盐酸川芎嗪的含量进行测定.方法采用十八烷基硅烷键合硅胶柱150mm×3.9mm,甲醇-水(6040)为流动相,检测波长为296nm,流速为1.0ml/min.结果该法能较好地分离被测组分和有关杂质,被测组分线性关系良好,回收率高.结论该法专属性好,简捷、快速、准确,适用于该产品质量分析检测.     

盐酸克林霉素乳膏剂的研制和质量控制

目的：建立克林霉素乳膏剂的制备方法和质量标准。方法：采用HPLC测定盐酸克林霉素含量，结果：该法有很好分离被测组分与其它杂质，线性范围5－2500μg（r=0.9985)，平均回收率98．72％，RSD＝1．52％。结论工艺简单，质量控制方法切实可行。     

高效液相色谱法测定盐酸西替利嗪口服液含量

目的：以高效液相色谱标法测定盐酸西替利嗪口服液含量。方法：采用硅胶色谱柱,乙腈－水－稀硫酸（９５：４．７：０．３）为流动相,检测波长２３０ｎｍ。结果：该法能较好地分离被测组分和苯甲酸钠,被测组分线性关系良好,回收率满意。结论：该法专属性好,快速,准确。     

气相色谱法测定头孢拉定残留溶剂

目的建立测试头孢拉定中残留溶剂甲醇、丙酮、二氯甲烷的气相色谱方法。方法三种残留溶剂均采用顶空进样法,以正丙醇作为内标物质;色谱柱：ZB-1型毛细管柱（30m×320μ,1μm）;柱温条件：0-4min120℃,以20℃／min的速度升到180℃,以180℃维持3min。结果头孢拉定中各被测组分均有很好的分离度,各纽分在一定范围内线性关系良好,精密度和准确度良好,三纽分低、中、高浓度的平均加样回收率分别为96．13％、99．01％、102．42％。结论本方法操作简单、用时短,可用于测定头孢拉定残留溶剂甲醇、丙酮、二氯甲烷的含量。     

HPLC法测定小儿安散中磺胺脒及磺胺二甲嘧啶的含量

以HPLC同时测定小儿安散中磺胺脒（SG）及磺胺二甲嘧啶（SM2）的含量。用C18柱,水-甲醇-冰醋酸（69：30：1）为流动相,检测波长为265nm。该法能很好地分离被测组分。被测组分的线性关系良好。回收率满意,该法简便可靠,重现性好。     

HPLC法测定卡巴匹林镁结构中阿司匹林的含量

目的：以ＨＰＬＣ外标法测定卡巴匹林镁结构中阿司匹林含量。方法：采用ＹＷＧ－Ｃ１８柱,冰醋酸－甲醇水（２．５：５４：５６）为流动相,检测波长２５４ｎｍ。结果：该法能较好地分离被没组分和有关杂质,被 没组分红性关系良好,回收率满意。结论：该法专属性好,快速、准确。     

HPLC法测定去氢表雄酮片的含量

目的 :建立去氢表雄酮片剂的高效液相色谱 (HPLC)测定方法。方法 :采用 μ-BondapakC18 柱 ,以CH3OH∶H2O (75∶25)为流动相 ,检测波长为292nm。结果 :该法能较好地分离被测组分与有关杂质 ,含量线性范围为0 2～1.0mg/ml,r=0.9999。结论 :该法简便、准确。     

HPLC法测定复方依那普利片累计溶出度

目的：复方依那普利药物中的有效成分为马来酸依那普利与氢氯噻嗪，本研究采用HPLC法测定复方依那普利的累计溶出度。方法：采用LUNAC18柱，甲醇－乙醚－三乙胺－水（3：0．025：0．01：20）为流动相，检测波长为215nm和272nm。结果：含量测定方法较好地分离被测组分和有关杂质，被测组分的线性关系很好，回收率满意，溶出度为90％以上。结论：此质量标准能很好地控制成品质量。     

布洛芬精氨酸盐注射液的制备及稳定性考察

目的:制备布洛芬精氨酸盐注射液并对其进行稳定性考察。方法:优化处方工艺后对布洛芬精氨酸盐注射液进行稳定性考察。采用反相高效液相色谱法测定布洛芬含量。结果:影响因素试验、加速试验及长期试验结果表明,布洛芬精氨酸盐注射液稳定。结论:布洛芬精氨酸盐注射液处方设计合理,工艺可行,质量稳定。     

盐酸精氨酸与醋酸精氨酸对机体酸碱平衡影响的实验研究

目的 :观察盐酸精氨酸与醋酸精氨酸对严重创伤后机体酸碱平衡的影响。方法 :采用30 %Ⅲ°烧伤家兔及正常大鼠灌喂模型 ,随机分为盐酸组和醋酸组 ,分别灌喂盐酸精氨酸和醋酸精氨酸 ,剂量为2 4g/(kg·d) ,连续7d。观察两种药物对烧伤大白兔及正常大鼠酸碱平衡和氯离子代谢的影响。结果 :两组正常大鼠连续用药7d后 ,反映酸碱平衡的各项指标及血浆氯离子水平无明显改变(P>0 05) ;烧伤家兔用药7d后盐酸组出现代谢性酸中毒 ,血浆氯离子含量也明显增高 ,而醋酸组变化不明显。结论 :严重烧伤家兔长时间大剂量应用盐酸精氨酸可导致高氯性酸中毒 ,应用醋酸精氨酸未造成明显不良反应 ,两种药物对正常大鼠均未产生不利影响。     

Arginine modulated cyclosporine-induced immune suppression in rats transplanted with gastric cancer cells

BACKGROUND: The incidence of cancer is significantly increased in kidney transplant patients receiving cyclosporine treatment. It has been reported that arginine can modify cyclosporine-induced nephrotoxicity in rats. Whether arginine interfered with cyclosporine-induced immune suppression in tumor transplant is not clear. MATERIALS AND METHODS: Male Wistar rats were inoculated subcutaneously with human gastric cancer SC-M1 cells and separated into 4 groups; control, cyclosporine, cyclosporine plus arginine and cyclosporine plus glycine groups. The growth of SC-M1 tumor was monitored on 4, 7, 10, 14 and 21 days after tumor implant. In another set of experiments, the rats were separated into control, cyclosporine, arginine and cyclosporine plus arginine groups. After treatment for one week, mononuclear cells were collected and stained with anti-rat CD3 antibody followed by flowcytometric analysis. On the other hand, splenocytes from each group of rats were stimulated with phyto-hemaglutinin (PHA) to determine their DNA synthesis by 3H-thymidine uptake assay. RESULTS: The SC-M1 tumors in the cyclosporine-treated rats were larger than that of the arginine plus cyclosporine group. Although SC-M1 tumors were eventually rejected in Wistar rats, the duration of detectable SC-M1 tumors in cyclosporine-treated rats was longer than that of rats treated with arginine plus cyclosporine. More infiltrating inflammatory cells were detected at an early stage of tumor rejection in rats treated with arginine plus cyclosporine than in cyclosporine-treated rats. In vitro analysis of PHA-stimulated splenocyte proliferation showed that arginine activated lymphocyte proliferation while cyclosporine inhibited lymphocyte proliferation. Arginine significantly interfered with cyclosporine-induced growth inhibition of PHA stimulated lymphocytes (p = 0.0039). CONCLUSION: Using a tumor transplant model, we have found that dietary supplements of arginine interfered with cyclosporine-induced immunosuppression in rats. The antagonistic effect between arginine and cyclosporine on immune suppression is worthy of further investigation in organ transplant patients.     

Development and validation of a high-resolution capillary electrophoresis method for multi-analysis of ragaglitazar and arginine in active pharmaceutical ingredients and low-dose tablets

A selective, sensitive and robust capillary electrophoresis (CE) method has been developed and validated for multi analysis of ragaglitazar (also known as NNC 61-0029 or DRF 2725) and its counter ion arginine in Active Pharmaceutical Ingredients (API) and low-dose tablets (0.5, 1.0 and 2.0 mg). The method covers a total number of 12 analyses for the API and tablets: assay and identification of ragaglitazar and arginine, chiral purity of ragaglitazar and purity of ragaglitazar. After a simple extraction of samples with acetonitrile and 0.01 M sodium hydroxide (10:90), separation was performed using a combination of two cyclodextrins; sulfobutylether-beta-cyclodextrin (SB-beta-CD) and dimethyl-beta-cyclodextrin (DM-beta-CD) in the electrolyte. The method showed good specificity and could separate and detect ragaglitazar, the distomer (the (+)-enantiomer) and arginine. The LOQ was found to be 0.10%, corresponding to 0.2 ng (0.5 microg/ml) for ragaglitazar and the distomer. Linearity was observed to be from 0.5 to 15 microg/ml (range 0.2-60 ng) and 400-600 microg/ml (range 1603-2404 ng) for ragaglitazar and 166-250 microg/ml (range 668-1000 ng) for arginine. The accuracy (as percent recovery) for ragaglitazar was found to be 101-106% (at 400-600 microg/ml), 101-125% (at 0.5-15 microg/ml) and for arginine 97-101% (at 166-250 microg/ml). The repeatability for the detection of peaks as R.S.D. was found to be as follows, ragaglitazar: 0.05%, distomer: 1.01%, largest single impurity: 5.84%, total impurities: 0.90% and arginine: 2.00%. The intermediate precision for the detection of peaks as R.S.D. was found to be as follows, ragaglitazar: 0.63%, distomer: 1.98%, largest single impurity: 5.22%, total impurities: 13.17% and arginine: 3.50.     

精氨酸对治疗性内镜逆行胰胆管造影后急性胰腺炎的预防作用

目的 :探讨精氨酸对治疗性内镜逆行胰胆管造影 (ERCP)后急性胰腺炎的预防作用。方法 :173例胰管均显影的患者随机分成治疗组 (A组 ,n =87)和对照组 (B组 ,n =86 ) ,A组治疗前、后静滴精氨酸 ,B组除不用精氨酸外 ,其他处理方法同A组。结果 :治疗性ERCP后高淀粉酶血症发生率 ,A组和B组分别为 2 7 6 %和 6 5 1% (P <0 0 1) ,急性胰腺炎发生率分别为2 3%和 11 6 % (P <0 0 5 )。结论 :精氨酸对治疗性ERCP后急性胰腺炎有明显的预防作用。     

AccQ-Tag法测定复方精氨酸胶囊中精氨酸的含量

目的：建立测定复方精氨酸胶囊中精氨酸含量的AccQ—Tag法^[1,2,3]。方法：以6-氨基喹啉-N-羟基琥珀酰亚胺基甲酸酯(AQC)为衍生剂，与复方精氨酸胶囊中精氨酸柱前定量衍生，用Waters HPLC仪，AccQ—Tag^TM氨基酸分析柱，以pH4．95醋酸钠缓冲液为流动相A，乙腈—水(3：2)为流动相B，进行梯度洗脱，检测波长为248nm。结果：线性范围：0．1006～0．9054μg，r=0．9995(n=5)。回收率：99．7％，RSD0．38％(n=5)。结论：本法快速、简便，辅料无干扰，结果满意。     

精氨酸布洛芬糖浆与布洛芬片剂人体药动学及生物等效性比较

目的:比较精氨酸布洛芬糖浆与布洛芬片在健康人体中的药动学及生物等效性。方法:采用液相色谱法测定18位健康男性受试者交叉服用精氨酸布洛芬糖浆和布洛芬片后的血浆中布洛芬浓度。结果:糖浆剂的药动学参数为:AUC_(0-10)=(150±s 17)mg·h·L~(-1),C_(max)=(47±9)mg·L~(-1),t_(max)=(0．6±0．3)h;布洛芬片剂的药动学参数为:AUC_(0-10)=(136±13)mg·L~(-1),c_(max)=(28±4)mg·L~(-1),t_(max)=(2．7±1．0)h,相对生物利用度为 (98±7)％。结论:精氨酸布洛芬糖浆和布洛芬片生物等效。     

柱前衍生化法测定血浆中醋酸精氨酸的浓度

目的:建立柱前衍生化高效液相色谱法测定血浆样品中醋酸精氨酸浓度的方法。方法:衍生剂为2,4—二硝基氟苯,色谱柱为氨基酸分析专用ODS色谱柱,流动相为50%乙腈-0.1mol/L醋酸钠溶液(29∶71),流速为1.2ml/min,检测波长为360nm,柱温为30℃。结果:醋酸精氨酸检测浓度线性范围为10~160μg/ml(r=0.9 998),高、中、低3种浓度血浆样品的回收率分别为(96.64±9.69)%、(90.94±4.70)%、(92.72±4.48)%,精密度<3.91%。含药血浆在冰冻条件(—24℃)下至少可以稳定15d。结论:本法简便可行,适用于醋酸精氨酸的血药浓度监测及其药动学研究。     

不同剂量精氨酸强化的肠外营养对胃肠癌患者术后免疫功能的影响

目的:探讨不同剂量精氨酸(Arg)强化的肠外营养(TPN)对胃肠癌患者术后免疫功能的影响.方法:选择90例胃肠癌患者,术后分别给予肠外营养支持,随机分为对照组(常规TPN,30例),试验Ⅰ组(TPN+Arg 15 g,30例)和试验Ⅱ组(TPN+Arg 30g,30例),分析术前术后不同时期白蛋白、总蛋白、C3、C4、CD4+ 、CD8+、CD4+/CD8+等免疫功能指标变化.结果:与对照组相比,Arg强化的TPN试验组患者免疫功能在术后第4天均有明显改善(P<0.05),随着精氨酸剂量的增加,总蛋白、CD4+ 、CD8+、CD4+/CD8+等指标改善更为显著(P<0.01).结论:精氨酸强化的TPN能提高胃肠癌患者术后免疫功能,添加精氨酸30 g优于15 g.     

慢支灵联合盐酸精氨酸方案治疗慢性支气管炎246例临床研究

目的：探讨慢支灵联合盐酸精氨酸方案在治疗慢性支气管炎及其所致酸碱失衡等并发症的有效性及安全性。方法：将本院246例慢性支气管炎患者随机分为两组,A组（对照组）采用常规抗感染平喘等对症支持治疗;B组（治疗照组）在常规治疗基础上采用慢支灵联合盐酸精氨酸治疗。结果：治疗后两组患者动脉血气酸碱指标及肺功能指标差异均具有统计学意义（P〈0.05）;A、B两组治疗总有效率及平均住院时间分别为84.55%、（16.6±7.4）d及93.50%、（11.3±6.8）d,两指标之间差异均具有统计学意义（P〈0.05）。结论：慢支灵联合盐酸精氨酸中西医结合的方案治疗慢性支气管炎,可更稳定的维持患者酸碱平衡、明显改善肺功能、缩短住院时间,具有优越的疗效,可提高患者生活质量。