吸收度线性组合分光光度法测定呋麻滴鼻液的含量

本文应用吸收度线性组合分光光度法,不经分离直接测定呋麻滴鼻液的含量。以251、257及375nm 波长为测试点,分别在各点测定呋喃西林和盐酸麻黄素混合液的吸收度,并通过单测点和线性组合,计算两者的含量。其回收率分别为100.72%(cv=0.65%)和100.89%(cv=0.59%)。     

吸收度线性组合分光光度法测定复方氯霉素醇溶液的含量

应用吸收度线性组合分光光度法,不经分离直接测定复方氯霉素醇溶液中氯霉素、水扬酸的含量。于276,278,280,296,298,300nm 波长处分别测定吸收度值,通过线性组合计算氯霉素和水扬酸的含量。其平均回收率分别为99.80%(CV=0.40%)100.36%(CV=0.40%)     

吸收度线性组合分光光度法测定灭痤霜中替硝唑和氯霉素的含量

取替硝唑、西咪替丁和氯霉素制成霜剂,以水溶解后采用吸收度线性组合分光光度法,在波长264nm,277nm,317nm处分别测定其吸收度,并通过单测点和线性组合计算替硝唑和氯霉素的含量.结果二者回收率分别为98.57%(RSD=0.53%)和98.95%(RSD=1.57%).     

吸收度线性组合法测定硫酸阿托品滴眼液的含量

本文应用吸收度线性组合分光光度法,不经分离直接测定硫酸阿托品滴眼液的含量。以239、258及275nm波长为测试点,分别在各点测定硫酸阿托品和尼泊金酯混乙合液的吸收度,通过各点的线性组合,计算硫酸阿托品的含量,其平均回收率为99.66%(CV=0.66%)。     

吸收度线性组合法测定硫酸阿托品滴眼液的含量

本文应用吸收度线性组合分光光度法,不经分离直接测定硫酸阿托品(Atropine Sulfate)滴眼液的含量。以239、258及275nm波长为测试点,分别在各点测定硫酸阿托品和尼泊金乙酯混合液的吸收度,通过各点的线性组合,计算硫酸阿托品的含量,其回收率为99.66％(CV％=0.66)。     

分光光度线性组合法测定硝酸毛果芸香碱滴眼液的含量

目的建立测定硝酸毛果芸香碱滴眼液含量的方法。方法应用分光光度线性组合分光光度法,不经分离直接测定硝酸毛果芸香碱、对羟基苯甲酸乙酯的含量,在208、210、256nm波长处分别测定吸收度,通过线性组合和单测分别计算两者的含量。结果硝酸毛果芸香碱在5~25μg·mL-1;对羟基苯甲酸乙酯在1~6μg·mL-1有良好的线性关系,平均回收率分别为99.45%(RSD=0.46%)、99.56%,(RSD=0.55%)。结论该方法简便、快速、准确、可用于该制剂的质量控制。     

吸收度线性组合分光光度法测定盐酸普鲁卡因注射液含量

本文采用吸收度线性组合分光光度法测定盐酸普普卡因注射含量,以磷酸盐缓冲液(pH6.5)为溶剂,以265、275及291nm波长为测试点测定吸收度,计算含量,其回收率为99.9%,(CV=0.36%)。本法具有操作简便、快速、结果准确可靠且能消除PABA干扰的特点。     

吸光度线性组合分光光度法测定呋磺胶囊的含量

目的:建立吸光度线性组合分光光度法测定呋磺胶囊中呋喃西林和磺胺嘧啶含量的方法.方法:应用吸光度线性组合分光光度法,不经分离直接测定呋磺胶囊中呋喃西林和磺胺嘧啶的含量.以260 nm、264 nm、375 nm为测定波长,分别在各点测定呋喃西林和磺胺嘧啶混合液的吸光度,通过线性组合计算磺胺嘧啶含量,用单波长测定呋喃西林含量.结果:平均回收率分别为99.98%、RSD=1.34%和99.94%、RSD=0.84%.结论:本方法简便、快捷,结果准确,适用于该制剂的质量分析检验.     

吸收度线性组合法测定盐酸乙基吗啡滴眼液的含量

本文应用吸收度线性组合法,不经分离直接测定盐酸乙基吗啡滴眼液的含量。以258、282、283及284nm波长为测试点,分别在各点测定盐酸乙基吗啡和尼泊金乙酯混合液的吸收度,通过各点的线性组合,计算盐酸乙基吗啡的含量。其回收率为100.12%.CV%=0.21%.本方法是测定盐酸乙基吗啡滴眼液的新方法,具有快速、准确的特点。     

吸收度线性组合分光光度法测定氯地滴眼液的含量

吸收度线性组合分光光度法是在安登魁教授指导下，由中国药科大学孙涛老师提出来的一种新的计算分光光度法。本文报告氯地滴眼液的含量测定，就足成功地利用该法的一个例证。经试验，以242、278及300nm波长为测试点，不经分离分别在各点测定氯霉素和地塞米松磷酸钠混合液的吸收度，计算两者的含量。平均回收率分别为99．46％(CV=0．40％，n=7)和100．13％(CV=0．45，n=7)。     

GC测定二-(2,6-二氟苯甲酰异羟肟酸)二正丁基合锡中有机溶剂残留量

目的建立原料药二-（2,6-二氟苯甲酰异羟肟酸）二正丁基合锡中的有机溶剂残留量的测定方法。方法采用毛细管气相色谱法,FID检测器,DB-1毛细管柱,柱温50℃,进样口温度200℃,检测器温度220℃,流速为2.0 mL.min-1,分流比为50∶1,以1,2-二氯乙烷为内标测定溶剂残留量。结果甲醇、正己烷、甲苯在考察的浓度范围内线性关系良好,线性范围分别为9~375μg.mL-1（r=0.999 8）,0.87~36.25μg.mL-1（r=0.999 7）,2.67~111.25μg.mL-1（r=0.999 8）,平均回收率分别为99.1%（RSD=2.5%）、98.3%（RSD=2.7%）、99.7%（RSD=1.3%）。结论本方法快速、简单、结果准确,可用于二-（2,6-二氟苯甲酰异羟肟酸）二正丁基合锡中的有机溶剂残留量的测定。     

Automated flow-injection spectrophotometric determination of catecholamines (epinephrine and isoproterenol) in pharmaceutical formulations based on ferrous complex formation

A novel automated flow-injection spectrophotometric method for the determination of catecholamines (epinephrine and isoproterenol) has been developed based on the formation of their coloured complexes with Fe(II) in aminoacetic-carbonate buffer pH 8.3 and measuring of the absorbance peaks at the lambda(max) of 530 nm. A fully automated FIA system controlled by home-made software (FIA-MOD) was used for optimising the chemical and manifold parameters and running of routine measurements. The calibration graph was linear in the range of 5-200 mg l(-1) for epinephrine with an RSD of 0.24% (n = 5; c = 150 mg l(-1)) and 10-300 mg(-1) for isoproterenol with an RSD of 0.13% (n = 5; c = 200 mg l(-1)). Measurement throughput was 120 h(-1) ensuring a sample throughput of 40 h(-1) analysed in triplicate. Common excipients for tablets and injections were found not interfering. The proposed method was applied for the assay of various commercial pharmaceutical formulations containing epinephrine and isoproterenol and for the content uniformity test for the isoproterenol tablets. The assay results with RSD 2-4% (n = 3) were comparable with those obtained with the official USP XXIII methods (mean difference 1.9%).     

Optical purity determination of (<Emphasis Type="Italic">S</Emphasis>)-lbuprofen in tablets by achiral gas chromatography

An optical purity test was indirectly performed on (S)-ibuprofen as its diastereomeric (R)-(+)-1-phenylethylamide derivative using achiral gas chromatography (GC). The method for the determination of trace (R)-ibuprofen (optical impurity), within the range 1.0 to 50 ng, from a racemic ibuprofen standard was linear (r = 0.9997) with acceptable precision (% RSD < or = 5.3) and accuracy (% RE = 0.7 - -3.9). Similar results were obtained with the method validation for the quantification of (S)-ibuprofen within the range 0.1 to 2.0 microg using a (S)-ibuprofen standard. When applied to seven different commercial (S)-ibuprofen products, their optical purities (98.7 - 99.1%) were determined with good precision (% RSD < or = 4.0).     

血凝仪-APTT法测定肝素的效价

目的:建立一种基于血液凝固分析仪测定活化部分凝血活酶时间(APTT)的肝素生物测定法(简称血凝仪-APTT法)。方法:将高、中、低浓度的肝素钠标准品和供试品分别与血浆混和,用血液凝固分析仪测定各含药血浆的活化部分凝血活酶时间(APTT),结果进行对数转换后,按量反应平行线3.3法计算供试品的效价。结果:对数凝血时间与肝素钠的浓度在0.7～3 IU.mL-1范围内线性关系良好(r=0.9965);当供试品的测得效价与估计效价的比值在80%～120%范围内时,血凝仪-APTT法的测定结果准确可靠,重复性(RSD=1.45%,n=6)及中间精密度(RSD=1.61%,n=6)良好。以兔全血法、羊血浆法和血凝仪-APTT法分别测定同一批肝素钠供试品的效价(IU.mg-1,n=3),结果依次为207.56±6.87,205.59±3.62,202.79±2.08,无显著性差异(P>0.05);兔全血法和血凝仪-APTT法的可信限率(%,n=3)分别为8.51±0.77和2.63±0.21,具有显著性差异(P<0.01)。使用不同仪器测定样品效价的结果基本一致。结论:血凝仪-APTT法与兔全血法和羊血浆法的效价测定结果一致,可信限率比兔全血法更低。该法操作简便,客观准确,重复性好,精密度高,适用于不同仪器,可以用于肝素钠生物效价的测定。     

HPLC-MS法测定首乌丸中五种蒽醌类成分的含量

目的建立首乌丸中芦荟大黄素、大黄酸、大黄素、大黄酚以及大黄素甲醚等五种蒽醌类成分的含量测定方法。方法 HPLC-MS联用法对首乌丸中五种蒽醌类物质的含量同时测定。色谱条件为:Phenomenex Luna C18(3μm,150 mm×2 mm)柱,流动相:甲醇-5 mmol/L醋酸铵溶液(90∶10),流速:0.2 mL/min,电喷雾型质谱检测器。结果大黄酸、芦荟大黄素、大黄素、大黄酚、大黄素甲醚分别在0.18～56.6,0.016～10.03,0.024～14.94,0.18～11.33,0.011～6.85 ng范围内线性良好;r分别为0.999 8,0.999 9,0.998 8,0.999 9,0.999 9;水解前平均回收率分别为108.5%(RSD=0.93%),98.67%(RSD=1.57%),100.2%(RSD=0.69%),99.73%(RSD=1.27%),105.4%(RSD=1.54%);水解后平均回收率分别为99.67%(RSD=1.12%),99.21%(RSD=1.78%),98.94%(RSD=1.23%),98.32%(RSD=2.08%),96.10%(RSD=2.67%)。结论此法简便、准确、快捷,可用于首乌丸的质量控制。     

回春至宝口服液质量标准的研究

本文采用薄层层析法对回春至宝口服液中红参、鹿茸、淫羊藿的有效成分进行定性；以ＨＰＬＣ法对主要成分之一的淫羊藿内的有效成分淫羊藿甙进行含量测定，方法准确、灵敏、重现性好，回收率达９８．９７％，ＲＳＤ＝１．５３％。     

气相色谱法测定恩替卡韦原料药中有机溶剂残留量

目的建立毛细管气相色谱法测定抗病毒原料药恩替卡韦中的有机溶剂残留量。方法采用DB-624毛细管色谱柱,FID检测器。载气为N2,流速为2ml·rain-1,进样口温度250℃,检测器温度为250℃。结果甲醇、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃、三乙胺、甲苯和苯甲醇的线性范围分别为0．06018～0．6018g·L-1（r=0．9973）、0．01202～0．1202g·L-1（r=0．9968）、0．00578～0．0578g·L-1（r=0．9972）、0．10348～1．0348g·L-1（r=0．9972）、0．01706-0．1706g·L-1（r=0．9968）、0．10126～1．0126g·L-1（r=0．9957）、0．01806-0．1806g·L-1（r=0．9983）和0．10074～1．0074g·L-1（r=0．9993）;平均回收率（n=9）分别为98．6％（RSD：2．36％）、95．5％（RSD=5．98％）、96．9％（RSD=4．36％）、100．5％（RSD=2．02％）、102．3％（RSD=3．86％）、100．1％（RSD=1．56％）、102．4％（RSD=1．88％）、99．4％（RSD=1．63％）。结论该方法操作简便、准确、灵敏度高、重复性好,适用于恩替卡韦原料药中有机溶剂残留量的测定。     

裙带菜多糖中硫酸基含量的测定

目的:采用硫酸钡比浊法测定裙带菜多糖中硫酸基的含量,并对测定方法进行了研究。结果:用紫外可见分光光度法检测最大吸收波长为360nm,在0-24μg/mL范围内线性关系良好(r=0.9997)。此方法的精密度良好(RSD为2.9%),具有较好的重复性(RSD为2.58%),同一样品在10-40min内的检测值比较稳定,回收率为(95.75±2.56)%。经测定,裙带菜多糖的硫酸基含量为10.58%。结论:该方法应用于裙带菜多糖硫酸基含量时结果比较准确,处理速度快,并且灵敏度较高。     

A method for routine analysis of recombinant immunoglobulins (rIgGs) by capillary isoelectric focusing (cIEF)

A capillary isoelectric focusing (cIEF) method was developed for routine analysis of recombinant immunoglobulins (rlgGs). The cIEF method used a dimethyl siloxane-coated capillary and a separation matrix of 2% ampholytes in 0.4% methylcellulose (MC). The rIgGs, and internal pI marker protein standards, were mixed with carrier ampholyte in MC, focused using high voltage, and then the protein bands were mobilized past a UV detector by simultaneous application of low pressure and voltage. Qualitatively and quantitatively equivalent rIgG focusing profiles were obtained via cIEF and gel-based IEF, with individual isoform peak area percentages and calculated peak pI values being comparable for the same samples. Linear relationships were obtained for peak area response versus sample concentration, and for the pI gradient developed between the internal pI marker standards. The relative standard deviation (RSD) in rIgG peak areas was less than 2% intra-day and less than 8% inter-day (72 h). The RSD for the mobilization times of rIgG peaks was less than 1% intra-day and less than 3% inter-day (72 h). There was no observed decrease in the performance of the capillary over 150 analyses. cIEF offers several important advantages over gel IEF, e.g. direct, quantitative detection of proteins by intrinsic UV absorbance at 280 nm, rapid analyses ( < or = 30 min), capability of automation, and one-step, electronic data analysis and archival. These data demonstrate the superiority of the cIEF method for routine analysis of rIgGs.     

佛波双酯注射液(TPA)含量测定方法改进

目的 对佛波双酯注射液的含量测定方法进行改进提高.方法 采用HPLC法测定佛波双酯注射液的含量及有关物质,色谱柱由Kromasil KR100-5 c18柱(250 mm×4.6 mm,5 μm)改为Shim-pack PA-DEAE 柱(固定相为二乙氨乙基,规格20 mm × 10 cm,10 μm),流动相由:乙腈-甲醇-水(45:45:10)改为乙腈-甲醇-水(60:35:5),流速为:1 ml/min^-1,检测波长为:232nm.结果 改进后用HPLC法测定佛波双酯注射液中佛波双酯的含量,佛波双酯在浓度33.5～354.4 μg/ml范围内,线性关系良好(r=0.99998);低、中、高3种浓度的方法回收率分别为100.8%、100.6%和100.9%,RSD均小于1.8%(n=3),平均回收率为100.8%,RSD为1.46.结论 本实验方法较原来的含量测定方法更简便、准确,灵敏,线性范围有所提高,相关程度增大,RSD值较原方法更精确,可用于佛波双酯注射液的含量测定,能更有效控制产品质量.