文章建立了测定保健品中维生素B1含量的高效液相色谱-柱后衍生法.方法采用色谱柱:UltimateXB-C18(4.6mm×150mm,5μm);流动相:(0.01％辛烷磺酸钠+1.5％乙酸+5％甲醇+0.12％三乙胺)-甲醇(65:35);流速:1.0 mL/min;柱温:35℃;检测波长:Ex=375nm,Em=435nm.研究发现该柱后衍生法测定同一样品中维生素B1含量得到的峰面积是柱前衍生法测定结果的1.6-18.8倍,维生素B1含量在0.01-32μg/mL范围内线性良好,R2=0.999,检出限为1 ng/mL.该方法灵敏、简便、准确,重现性好,可用于保健品中维生素B1含量的测定.

OBJECTIVE:To investigate the compatibility stability of Ulinastatin for injection with 2 commonly used solvents in the infusion pump.METHODS:After Ulinastatin for injection 500 000 U was respectively added into 0.9％ Sodium chloride injection and 5％ Glucose injection 50 mL,the appearance of the mixture at 25 ℃,37 ℃ were observed at 0,1,2,4,8,12,24 h,re spctively,pH value and the number of insoluble particles were measured.The relative percentage of ulinastatin in the mixture was determined by HPGFC.RESULTS:Under this condition,the appearance and pH value of the mixture had no significant change within 24 h;the number of particles ≥10 μm was lower than 25 particle/mL,and that ≥25 μm was lower than 3 particle/mL,which was in line with the pharmacopeia standard.The relative percentage of ulinastatin within 24 h ranged 99.45％-102.55％.CONCLUSIONS:After mixed with 0.9％ Sodium chloride injection and 5％ Glucose injection,Ulinastatin for injection keep stable within 24 h at 25 ℃,37 ℃ and can be used for continuous administration in the infusion pump.

目的:用HPLC法探索7种糖尿病病人常用药与木糖醇注射液的配伍稳定性,为临床用药提供参考.方法:建立HPLC法测定硫辛酸注射液、注射用埃索美拉唑钠、注射用血栓通、丹参酮ⅡA磺酸钠注射液、氨溴索注射液、氨茶碱注射液、地塞米松磷酸钠注射液7种药品在木糖醇注射液中的含量.观察配伍液在室内见光或避光条件下,放置不同时间后的外观,测定pH值及含量.结果:硫辛酸注射液在室内见光条件下,0～8h内配伍液由无色澄清变为黄色,pH值由7.84降为5.76,6h后含量＜90％;在避光条件下,pH值无明显变化,8h内含量为98.53％.注射用埃索美拉唑钠无论是避光还是室内见光条件,在6h时配伍液均由无色澄清变为微黄色,pH值均略有下降,8h后含量分别是97.33％、96.22％.其他5种药品与木糖醇注射液配伍后,在避光条件和室内见光条件下,8h内配伍液的pH值、颜色、澄清度均无明显变化,含量测定结果均＞98％.结论:硫辛酸注射液见光易分解,建议临床避光下使用.注射用埃索美拉唑钠与木糖醇注射液配伍6h内可安全使用.其他5种药品与木糖醇注射液配伍8h内稳定,可配伍使用.

目的：建立高效液相凝胶过滤色谱法测定注射用乌司他丁中乌司他丁的含量。方法色谱柱：凝胶柱TSKgel G3000SWxl(7.8 mm×300 mm,5μm)；流动相：[0.001 mol·L-1磷酸二氢钠-0.001 mol·L-1磷酸氢二钠(39：61)]-乙腈(90：10)；流速0.7 mL·min-1；检测波长280 nm；柱温25℃；进样量20μL。结果乌司他丁的检测质量浓度线性范围为0.78125~50.00 U(r =0.9999)；低、中、高剂量样品平均回收率分别为100.32%,100.17%,100.21%, RSD 分别为0.633%,0.568%,0.414%(n=3)。结论该法简便、快速,结果准确,可用于乌司他丁的含量测定。

目的 考察注射用二丁酰环磷腺苷钙与肌苷注射液的配伍稳定性.方法 采用HPLC法检测注射用二丁酰环磷腺苷钙和肌苷注射液与常见溶媒配伍后的含量变化,同时观察并检测配伍溶液的外观及pH值.结果 室温条件下,8h内配伍溶液的pH及肌苷的含量无显著变化.二丁酰环磷腺苷钙的含量不断下降,且在葡萄糖氯化钠注射液中下降速度最快.结论 注射用二丁酰环磷腺苷钙与肌苷注射液存在配伍禁忌.

目的 采用HPLC法对3个厂家生产的注射用还原型谷胱甘肽进行含量测定.方法 采用Acclaim C18(250mm ×4.6 mm,5μm)色谱柱,以(26 mmol·L-1磷酸二氢钾,6 mmol·L-1辛烷磺酸钠,磷酸调pH =3.0)-甲醇(90∶ 10)为流动相,流速:1.0 ml ·min-1,检测波长:210 nm,柱温:30℃.结果 还原型谷胱甘肽在37.5～200 μg ·ml-1浓度范围内线性关系良好(r =0.9998).平均回收率为100.03％,RSD为1.29％.不同厂家注射用还原型谷胱甘肽的含量不同,均达到药典规定.结论 本法简便、专属性良好、准确可靠,可作为注射用还原型谷胱甘肽含量测定的方法.

目的:考察注射用丙帕他莫与β-内酰胺类药、质子泵抑制剂(PPI)的配伍稳定性.方法:采用高效液相色谱(HPLC)法测定丙帕他莫48 h内的含量变化,考察其pH值变化,并观察与β-内酰胺类药及PPI配伍后各溶液的外观变化.结果:丙帕他莫的水溶液不稳定,药物含量在7h内可降解至90％以下,pH值在3h内从5.37降至3.52,48 h后pH值降至1.87.丙帕他莫与β-内酰胺类药配伍3h时肉眼可观察到液体乳光,配伍12h时可观察到白色沉淀;与PPI配伍立即发生颜色的变化并逐渐形成深色沉淀.结论:丙帕他莫的水溶液稳定性差,与β-内酰胺类药物及PPI存在配伍禁忌.丙帕他莫临床上应现配现用,尽量在配伍1h内用完且不与其他药物进行配伍,输液前后应冲管.

目的 建立氨曲南与利巴韦林的含量测定方法,通过注射用氨曲南与利巴韦林注射液配伍后含量变化来考察其配伍的稳定性,进而为临床采用合理的配制方法提供参考依据.方法 在25℃和37℃条件下,将注射用氨曲南与利巴韦林注射液在100 ml 0.9％氯化钠注射液、5％葡萄糖注射液中配伍,测定溶液的pH值,采用HPLC法测定配伍液中氨曲南和利巴韦林的含量,定时观察溶液的颜色及澄明度.结果 本实验所建立的色谱条件对注射用氨曲南和利巴韦林注射液的检测专属性好,氨曲南、利巴韦林的线性范围分别在0.0125～ 0.2 mg ·ml-1(r=0.9999),0.006～0.1 mg·ml-1 (r =0.9999).25℃和37℃条件下,氨曲南和利巴韦林在0.9％氯化钠注射液和5％葡萄糖注射液中配伍后,溶液24 h内配伍液均无外观改变、pH值在5.4左右无明显变化、含量在95％以上、吸收峰的位置无变化,无其它吸收峰产生.结论 两种药物的结构稳定,在溶液中稳定性好,临床上可将两药配伍使用.

Objective To investigate a appropriate chromatography method for ALA and the stability of ALA in xylitol injection and fructose injection. Methods 600 mg ALA was added into 250 mL xylitol injection and fructose injection respectively at room temperature and dark conditions,pH value and visual appearance of the admixture were observed at immediate 1,2,4,6,8,12,24 h after ALA adding to the solvent. ALA concentrations were determined by the method of HPLC. Results The chromatography method established in this study was specific,ALA showed a good linear relationship within the range of 0. 06 ~2. 0 mg/mL ( r =0. 999 7 ) . The admixture showed clear and achromatic color in 24 h after adding into the 0. 9%NS,5%xylitol injection,and the pH value and ALA content showed no great change. pH value,colour,visual appearance of the admixture changed apparently after ALA adding into fructose injec-tion,and the degradation was rapid,the content of ALA was 89. 89%after 4 h. Conclusion ALA can be mixed with xylitol injection in clinical practice,but cannot be mixed with fructose injection.

Objective To explore the reason for white crystalline development in dual-channel infusion tube when combing β-lactams with pethidin and propacetamol in the micro-infusion pump. Methods The reason of incompatibility was explored by repeated simulating tests for the same drugs' combination. Results The white precipitation occurred in the dualchannel infusion tube when pethidine encountered β-lactams. Propacetamol for injection was unstable. Decomposition products of propacetamol lowered pH of the infusion to 3. 34 after drug combining for three hours. After the acid nonresistant drugs such as β-lactams were added to the infusion liquid,with pH dropped from 5. 37 to 1. 87 over 24 h,and white crystals gradually developed. Conclusion Propacetamol in the infusion pump should not be used as intravenous drip for a long time. If used,propacetamol should be infused alone. The infusion pump liquids containing Pethidine should not be infused with β-lactams simultaneously in the multi-channel infusion tube.

目的 考察亮菌甲素与6种常用输液的配伍稳定性及其荧光强度随溶剂pH值的变化情况.方法 采用高效液相色谱法测定亮菌甲素注射液与0.9％氯化钠注射液、5％葡萄糖注射液、10％葡萄糖注射液、葡萄糖氯化钠注射液、木糖醇注射液及乳酸钠林格注射液配伍后亮菌甲素的含量,采用pH测定仪测定其酸碱度变化,同时观察溶液的颜色及澄明度.配置不同pH梯度的缓冲盐溶液,考察亮菌甲素在不同pH环境下荧光强度的变化.结果 本实验所建立的色谱条件对亮菌甲素注射液的检测专属性好,亮菌甲素在5.0 ～ 80 μg/mL浓度范围内与其峰面积呈良好的线性关系(r2 =0.999 9).高、中、低3种浓度的平均回收率分别为103.72％(RSD=0.17％)、103.98％(RSD=0.01％)、103.67％(RSD=0.25％);6种配伍溶液在24 h时测得的药物含量均在98.61％ ～ 100.29％范围内.当溶液pH为5～8时,呈蓝色荧光黄色液体;pH为4～5时,肉眼观察微弱蓝色荧光;pH为2～4时,肉眼观察为无色透明液体,在紫外灯下可见微弱蓝色荧光.结论 亮菌甲素在不同pH值的溶媒中的荧光强度不同,荧光的强弱不影响药物的稳定性,该药物与6种常用输液配伍后24 h内稳定性良好.