舒必利及其片剂的比色测定法

目的：测定舒必利制剂中舒必利的含量,增加质量控制手段。方法：利用舒必利与７,７,８,８四氰基对二次甲基苯醌（ＴＣＮＱ）形成１∶１荷移络合物,应用比色法测定制剂中舒必利含量。结果：药物浓度在２～２６μｇ·ｍＬ－１范围内呈线性关系,样品回收率为９９１％～９９３％（ｎ＝３）。结论：方法简便、灵敏、准确,可做为该药制剂的含量测定方法。     

离子对高效液相色谱法测定注射用美洛西林钠—舒巴坦钠含量

目的：建立反相离子对高效液相色谱法测定注射用美洛西林钠－舒巴坦钠含量。方法：采用μＢｏｎｄａｐａｋＣ１８色谱柱,０００５ｍｏｌ·Ｌ－１氢氧化四丁基铵－乙腈（６８∶３２,ｐＨ５０±０１）为流动相,２３０ｎｍ为检测波长,３０℃柱温下对美洛西林和舒巴坦进行分离和测定。结果：能同时测定制剂中美洛西林和舒巴坦的含量。美洛西林在０２５～１５ｍｇ·ｍＬ－１,舒巴坦在０１２５～０７５ｍｇ·ｍＬ－１范围内,峰面积与其浓度呈良好线性关系（ｒ＝０９９９９）;平均回收率（ｎ＝５）美洛西林为９９７６％（ＲＳＤ＝０９２％）,舒巴坦为９９６６％（ＲＳＤ＝０８５％）。结论：该法简便、快速、准确,适用于该药品生产及临床应用中的质量监控。     

小儿速效感冒冲剂中对-乙酰氨基酚的测定

目的：通过试验以求快速测定小儿速效感冒冲剂主药的含量。方法：采用差式分光光度法（△Ａ）［１，２］测定小儿速效感冒冲剂中对－乙酰氨基酚的含量，并与亚硝酸钠法进行对照。结果：△Ａ平均回收率为９９３％，ＣＶ为０５０％（ｎ＝５），两法比较Ｐ＞００５，无显著性差异。结论：△Ａ法测定对－乙酰氨基酚含量可以排除其它组份干扰，快速准确。     

人工神经网络分光光度法用于增效联磺片三组分的同时测定

采用误差反传（ＢＰ）人工神经网络同时测定模拟增效联磺片三组分含量,磺胺嘧啶（ＳＤ）、磺胺甲基异恶唑（ＳＭＺ）、甲氧苄胺嘧啶（ＴＭＰ）的平均回收率和相对标准差分别为１０１０％、０６６％;９９４％、１１％;１００４％、１２％;且讨论了网络结构和参数对分析结果的影响     

Basic fibroblast growth factor protected forebrain against ischemia-reperfusion damage in rats

目的：研究碱性成纤维细胞生长因子（ｂＦＧＦ）对大鼠脑缺血再灌注损伤的影响．方法：电灼闭塞椎动脉并夹闭颈动脉，使大鼠前脑缺血２０分钟后，放开双侧颈动脉再灌．用高压液相色谱法测定纹状体中多巴胺（ＤＡ）类物质含量并用原子吸收分光光度法测定前脑中钠、钾含量．结果：再灌６小时后，纹状体中ＤＡ含量由对照的（９９±１６）μｇ·ｇ－１（蛋白）减少至（７０±２０）μｇ·ｇ－１蛋白；脑含水量由７７３４％±０１９％增加到７９６％±０６％；钠含量由（９３±０６）ｍｇ·ｇ－１（脑干重）增加到（１０５±０６）ｍｇ·ｇ－１（脑干重）．再灌开始后即刻静注ｂＦＧＦ４５μｇ·ｋｇ－１·ｈ－１共３ｈ可阻止ＤＡ的减少和水、钠含量的升高．组织学分析也表明ｂＦＧＦ可减轻神经元所受损伤．结论：ｂＦＧＦ可以保护神经细胞对抗脑缺血再灌损伤．     

两种指示剂法测定氯化钠含量结果比较

目的：比较两种指示剂法测定氯化钠含量。方法：采用吸附指示剂法（药典法）与铬酸钾指示剂法。结果：吸附法测定氯化钠含量（相当标示量％）为１００５９±０９０，ＲＳＤ（％）为０８９；铬酸钾法为１０１０１±０８５，ＲＳＤ为０８４，前者平均回收率为９９３±０９５，ＲＳＤ为０９６；后者为９９３±１０１，ＲＳＤ为１０２。结论：铬酸钾指示剂法具有终点明显、回收率高、测定结果准确，可作为氯化钠含量测定的简便易行方法     

高效液相色谱法测定双扑伪麻片中扑热息痛、盐酸伪麻黄碱、扑尔敏的含量

用高效液相色谱法,同时分离测定双扑伪麻片中扑热息痛、盐酸伪麻黄碱和扑尔敏的含量．线性范围：扑热息痛０２０～０８０ｇ／Ｌ,ｒ＝０９９９５;盐酸伪麻黄碱００１２～００４８ｇ／Ｌ,ｒ＝０９９９６;扑尔敏００００７２～０００２８８ｇ／Ｌ,ｒ＝０９９９２．平均回收率（ｘ±ｒｓｄ）％分别为：扑热息痛（１００２±１７）％;盐酸伪麻黄碱（９９６±１４）％;扑尔敏（９８４±２６）％．     

褶合光谱法测定复方替硝唑含漱剂含量

目的：研究测定复方替硝唑含漱剂含量的方法。方法：采用褶合光谱法不经分离直接测定替硝唑和醋酸氯己定的含量。结果：平均回收率和ＲＳＤ分别为９９９５％,０７４％;９９９３％,０５５％。结论：采用褶合光谱法不经分离直接测定复方中的两组分含量,方法简便、快速,结果准确。     

用紫外分光光度法测定注射用头孢唑啉钠含量

采用紫外分光光度法测定了注射用头孢唑啉钠含量．头孢唑啉钠浓度为１０～３０μｇ／ｍＬ时呈很好的线性关系，回归方程：Ａ＝００２８９Ｃ－０００７４；ｒ＝０９９９９（ｎ＝５），平均回收率为９９８％，ＲＳＤ＝０２％．     

分光光度法测定盐酸吗啉胍片含量并于非水滴定法比较

目的：用紫外分光光度法测定盐酸吗啉胍片含量。方法：按处方比例分别取马啉胍纯品和辅料在２００ｎｍ～３００ｎｍ波长范围内扫描，建立紫外吸收图谱。结果：盐酸吗啉胍在波长２３７ｎｍ处有最大吸收，而辅料在此无吸收。紫外法与非水法的回收率分别为９９８％，ＲＳＤ＝０５４（ｎ＝６）；９９８％，ＲＳＤ＝０５４（ｎ＝６）；９９９％，ＲＳＤ＝０４３（ｎ＝６）。变异系数分别为０５４７３％，０５４５９％，０４４２３％。结论：此法简便、快速、经济，与非水滴定法比较，结果基本一致     

Determination the content of gypsum fibrosum in Xiaokening tablets by powder X ray diffraction method

The research on the application of X-ray diffraction in the quantitative analysis of Chinese medicines is rare. The main reason is that the technical problems related to the internal standard and the selection of quantitative peaks are not well solved, and the accuracy and precision of the results are not satisfactory. This study employed the concept of mass absorption coefficient based on the internal standard method, and the full spectrum fitting and quantitative methods were used to solve the above technical problems. The sample was blended, the internal standard substance of zinc oxide was fully ground, and tablets were prepared by positive pressure method. Under certain instrumental conditions, the PXRD pattern was obtained by scanning. The percentage of gypsum fibrosum in Xiaokening tablet was obtained by quantitative analysis of full spectrum fitting internal standard by TOPAS software. The method was investigated by methodology. At the same time, the method was compared by ion chromatography, and SPSS software was used to make a significant t test on the results of the two methods. After the investigation, the average standard recovery rate of CaSO₄·2H₂O was 99.06% (RSD=3.02%); and the recovery rate for simulated samples was 96.7%. The method had good specificity. After statistical analysis, there was no significant difference between the new PXRD method and the traditional method of ion chromatography.     

HPLC assay of acetylsalicylic acid,paracetamol, caffeine and phenobarbital in tablets

This paper present a HPLC method for simultaneous determination of acetylsalicylic acid, paracetamol, caffeine and phenobarbital in tablets, using chromatographic system consisting a Bio Rad 18 01 solvent pump, Rheodine 71 25 injector and Bio Rad 18 01 UV-Vis Detector. Separation was achieved using Bio SiL HL C18, 5 microm, 250 x 4.6 mm column. Mixture of acetonitrile-water (25:75 v/v) adjusted to pH 2.5 with phosphoric acid was used as a mobile phase at a flow rate of 2.0 ml min(-1). UV detection was at 207 nm range 0.01 AUFS. Under the same conditions it was possible to determine the level of salicylic acid. The chromatographic parameters such as retention times, capacity factor, peak asymmetry, selectivity factor and resolution factor was determined. The validation parameters: linearity (r > 0.998), intra-day precision (RSD: 0.36-1.89%) and inter-day precision (RSD: 0.58-2.18%), sensitivity (LOD: 9 x 10(-5)-1.7 x 10(-4) mg ml(-1) and LOQ: 2.5 x 10(-4)-5.6 x 10(-4) mg ml(-1)), accuracy (recoveries: 98.35-99.14%) and reproducibility (recovery values: 98.74-102.08% for acetylsalicylic acid, 99.93-102.11% for paracetamol, 98.25-102.12% for caffeine and 98.15-102.3% for phenobarbital) (RSD: 1.21-1.85%) were found to be satisfactory. The proposed HPLC method has been applied for the determination of acetylsalicylic acid, paracetamol, caffeine and phenobarbital in Malophenum tablets. The obtained RSD values were within 0.99-1.21%. The developed method is rapid and sensitive and therefore suitable for routine control of these drugs in dosage form.     

高效液相色谱法测定苯巴比妥、苯妥英、卡马西平的血药浓度

目的 :建立 HPL C法测定抗癫药苯巴比妥 (PB)、苯妥英 (PT)、卡马西平 (CBZ)的血药浓度。方法 :反相柱 ODS- Hy-persil(4.6 m m× 10 0 mm ,5︼m ) ,流动相为甲醇∶水 (5 2∶ 48) ,流速 0 .8m l/ m in,紫外检测波长 2 5 4nm ,以上 3药互为内标。标本经 CH2 Cl2 提取 ,蒸干后用流动相重溶进样。结果 :PB、PT、CBZ的保留时间分别为 3.2 2、5 .5 7、6 .80 m in;最低检测浓度分别为 0 .2 5、0 .5、0 .0 5︼g/ m l;线性范围分别为 2 .5～ 40、2 .5～ 40、1.2 5～ 2 0︼g/ ml;相对回收率分别为 10 1.49%、10 4.19%、98.70 % ;日内 RSD分别为 1.81%、5 .94%、1.81% ;日间 RSD分别为 6 .0 6 %、3.35 %、3.96 %。结论 :本法具快速、灵敏、实用等优点。     

RP-HPLC同时测定冠心宁注射液中丹参素、原儿茶醛、阿魏酸、迷迭香酸和丹酚酸B的含量

目的:建立反相高效液相色谱法同时测定冠心宁注射液中丹参素、原儿茶醛、阿魏酸、迷迭香酸和丹酚酸B的含量。方法:采用Kromasil C18(4.6 mm×250 mm,5μm)色谱柱,流动相为乙腈(A)-0.05%三氟乙酸(B),梯度洗脱(0～65 min,2%A→30%A),流速0.8 mL.min-1,检测波长288 nm,柱温40℃。结果:丹参素、原儿茶醛、阿魏酸、迷迭香酸和丹酚酸B进样量分别在0.352～7.032μg(r=0.9999),0.080～1.594μg(r=0.9999),0.016～0.322μg(r=0.9999),0.057～1.133μg(r=0.9999),0.122～2.446μg(r=0.9999)范围内呈现良好的线性关系;平均回收率(n=6)分别为100.9%(RSD=1.5%),102.4%(RSD=0.9%),103.6%(RSD=0.9%),102.6%(RSD=2.0%),102.0%(RSD=2.1%);重复性试验,5个成分含量的RSD(n=6)均小于2.5%。结论:所建立的方法简便、准确,具有良好的重复性和稳定性,可用于冠心宁注射液的质量控制。     

HPLC法同时测定吴茱萸中吴茱萸碱、吴茱萸次碱与吴茱萸内酯的含量

目的:建立同时测定吴茱萸中吴茱萸碱、吴茱萸次碱与吴茱萸内酯含量的方法。方法:采用高效液相色谱法。色谱柱为迪马C1(8200mm×4.6mm,5μm),流动相为乙腈-0.04%庚烷磺酸钠溶液(48:52,V/V),流速为1.0mL·min-1,检测波长为225nm,柱温为35℃。结果:吴茱萸碱、吴茱萸次碱、吴茱萸内酯的进样浓度分别在5.38～53.80、5.02～50.20、10.30～103.00μg·mL-(1r均为0.9999)范围内与各自峰面积积分值呈良好线性关系;三者平均加样回收率分别为99.75%、97.66%、85.68%,RSD分别为0.67%、1.16%、1.54%(n=6)。结论:本方法简便、可行、重复性好,可用于吴茱萸中吴茱萸碱和吴茱萸次碱的含量测定;但吴茱萸内酯的回收率较低,需进一步改进其测定方法。     

HPLC法测定镇痛复方制剂阿司匹林萘磺酸右丙氧芬片含量及对其分解产物的定量检查

本文介绍了用高效液相色谱法测定阿司匹林、萘磺酸右丙氧芬片含量及其分解产物水杨酸含量的方法。采用 μ-BondapakC18 为固定相 ,0.02mol·L-1 磷酸二氢钾 -甲醇 -四氢呋喃(THF)(2:1:0.1)为流动相 ,紫外检测器于230nm波长处测定 ,方法准确可靠 ,对阿司匹林和萘磺酸右丙氧芬的回收率分别为99.25 %(RSD0.78 %)、99.7 %(RSD1.05 %)。由于阿司匹林不稳定 ,易分解成水杨酸 ,影响制剂质量。本方法的色谱条件可使阿司匹林、水杨酸、萘磺酸右丙氧芬完全分离 ,因此可同时用于水杨酸含量的检查。     

RP-HPLC同时测定大卫颗粒中绿原酸、黄芩苷、连翘苷、黄芩素和汉黄芩素的含量

目的:建立RP-HPLC法同时测定大卫颗粒中绿原酸、黄芩苷、连翘苷、黄芩素和汉黄芩素的含量。方法:采用Diamon-sil C18(200 mm×4.6 mm,5μm)色谱柱,以乙腈(A)-0.05%磷酸溶液(B)为流动相进行梯度洗脱(0～10 min,10%A→15%A;10～15 min,15%A→25%A;15～25 min,25%A→28%A;25～35 min,28%A→35%A),柱温35℃,流速1.0 mL.min-1,检测波长230 nm,进样量20μL。结果:绿原酸、黄芩苷、连翘苷、黄芩素和汉黄芩素5个成分质量浓度分别在2.80～28.0μg.mL-1(r=0.9992)、25.71～257.1μg.mL-1(r=0.9994)、0.71～7.1μg.mL-1(r=0.9995)、0.81～8.1μg.mL-1(r=0.9990)、0.50～5.0μg.mL-1(r=0.9992)的范围内与峰面积呈良好的线性关系;方法的平均回收率(n=9)分别为100.0%,99.0%,99.0%,99.9%,99.4%。结论:所建立的高效液相色谱测定法简便、准确,重复性好,专属性强,可用于大卫颗粒的含量测定质量控制。     

HPLC法测定胃炎康胶囊中芍药苷、盐酸小檗碱及甘草酸的含量

目的:以HPLC法同时测定胃炎康胶囊中芍药苷、盐酸小檗碱及甘草酸的含量。方法:采用Kromasil C18(250 mm×4.6mm,5μm)色谱柱,以乙腈-0.5%三乙胺水溶液(磷酸调pH 3.0)为流动相,梯度洗脱,流速1.0 mL.min-1,检测波长238nm,柱温30℃。结果:芍药苷、盐酸小檗碱及甘草酸线性范围分别为21.28～170.2,30.18～241.2,20.86～166.9 mg.L-1(r≥0.9993);平均加样回收率(n=5)分别为97.1%(RSD=1.2%),98.5%(RSD=2.0%),99.7%(RSD=0.87%)。结论:该方法操作简便,快速易行,结果准确可靠,可以作为胃炎康胶囊中芍药苷、盐酸小檗碱及甘草酸的含量测定方法。     

Quantification of carbamazepine, carbamazepine-10,11-epoxide, phenytoin and phenobarbital in plasma samples by stir bar-sorptive extraction and liquid chromatography

A sensitive and reproducible stir bar-sorptive extraction and high-performance liquid chromatography-UV detection (SBSE/HPLC-UV) method for therapeutic drug monitoring of carbamazepine, carbamazepine-10,11-epoxide, phenytoin and phenobarbital in plasma samples is described and compared with a liquid:liquid extraction (LLE/HPLC-UV) method. Important factors in the optimization of SBSE efficiency such as pH, extraction time and desorption conditions (solvents, mode magnetic stir, mode ultrasonic stir, time and number of steps) assured recoveries ranging from 72 to 86%, except for phenytoin (62%). Separation was obtained using a reverse phase C(18) column with UV detection (210nm). The mobile phase consisted of water:acetonitrile (78:22, v/v). The SBSE/HPLC-UV method was linear over a working range of 0.08-40.0mugmL(-1) for carbamazepine, carbamazepine-10,11-epoxide and phenobarbital and 0.125-40.0mugmL(-1) for phenytoin, The intra-assay and inter-assay precision and accuracy were studied at three concentrations (1.0, 4.0 and 20.0mugmL(-1)). The intra-assay coefficients of variation (CVs) for all compounds were less than 8.8% and all inter-CVs were less than 10%. Limits of quantification were 0.08mugmL(-1) for carbamazepine, carbamazepine-10,11-epoxide and phenobarbital and 0.125mugmL(-1) for phenytoin. No interference of the drugs normally associated with antiepileptic drugs was observed. Based on figures of merit results, the SBSE/HPLC-UV proved adequate for antiepileptic drugs analyses from therapeutic levels. This method was successfully applied to the analysis of real samples and was as effective as the LLE/HPLC-UV method.     

HPLC法测定华山参滴丸中东莨菪碱、阿托品及东莨菪内酯的含量

目的:建立HPLC法测定华山参滴丸中东莨菪碱、阿托品及东莨菪内酯的含量。方法:采用资生堂CAPCELL-PAK C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-甲醇-磷酸氢二钠缓冲液(15∶4∶81)为流动相,流速1.0 mL·min-1,东莨菪碱、阿托品检测波长210 nm(0～15 min),东莨菪内酯检测波长为344 nm(15.1～30 min),柱温30℃。结果:东莨菪碱、阿托品及东莨菪内酯的线性范围分别为0.04～3.95,0.04～4.10,0.05～0.54μg(r=0.9999);平均回收率(n=6)分别为97.58%(RSD=1.3%),98.65%(RSD=1.3%),98.42%(RSD=1.8%)。结论:本文方法简便、准确,可以用于华山参滴丸中东莨菪碱、阿托品及东莨菪内酯的含量测定。