盐酸左氧氟沙星注射液颜色检测的研究

目的：对盐酸左氧氟沙星注射液的溶液颜色检查进行了研究。方法：试验了样品与黄绿色标准比色液的颜色比较,同时确定了黄绿色标准比色液的最大吸收波长,将样品溶液进行了加速试验和浓缩,并将它们与原液同时进行了分光光度法测定。结果：样品与黄绿色标准比色液无法相等比较。颜色深过原液二倍多的试验溶液在450nm波长处测定的吸收度变化不大,无法达到控制质量的目的。结论：照分光光度法测定时,波长应改为430nm,吸收度可设定为“不得过0．07”。     

对中国药典1990年版二部附录中"溶液的颜色检查法"的补充

固体或液体药品的颜色差异在一定程度反映药品的质量变化。中国药典(1990年版)对固体颜色一般未做限度检查,对液体药品的颜色则采用了目视比色及紫外吸收的方法。在实践中发现不少药液的颜色与标准比色液色调不一致且对边缘产品采用目视法无法进行量化的科学区分。     

色差法测定溶液的颜色及其在药物分析中的应用

《中国药典》在2000年版附录中首次收载了色差法测定药品溶液的颜色,作为溶液颜色检查的第三法。如果用最简洁的语言概括此方法,就是应用色差计,以水作为参比物质,分别测定药品溶液和标准比色液与水的色差值,通过比较二者的大小,判断药品溶液颜色的合格与否。     

中美英三国药典标准比色液的对比与测定

目的:对中美英三国药典标准比色液的配制方法及不同测定方法所得的颜色参数进行对比,为进口药品检验和进口药品质量标准复核时颜色质量标准的制订提供参考。方法:采用《中国药典》2005版附录收载的目视比较法、紫外分光光度法、色差计法进行测定。结果:中英药典标准比色液之间有相似之处,但与美国药典标准比色液差别较大。     

国家食品药品监督管理局国家药品标准修订件XGB2008—002——阿莫西林钠

[修订] 【检查】溶液的澄清度与颜色取本品5份，各0．6g，分别加水5mL溶解后，溶液应澄清无色；如显浑浊，与1号浊度标准液（附录Ⅸ B）比较，均不得更浓；如显色，与黄色或黄绿色6号标准比色液（附录ⅨA第一法）比较，均不得更深。溶液初溶时可呈现短暂的粉红色。     

国家食品药品监督管理局国家药品标准修订件XGB2008—003——注射用阿莫西林钠

[修订] 【检查】溶液的澄清度与颜色取本品5瓶，按标示量分别加水制成每1mL中含0．1g的溶液，溶液应澄清无色；如显浑浊，与1号浊度标准液（附录ⅨB）比较，均不得更浓；如显色，与黄色或黄绿色6号标准比色液（附录ⅨA第一法）比较，均不得更深。溶液初溶时可呈现短暂的粉红色。     

注射用头孢拉定在25℃时的稳定性研究

目的考察注射用头孢拉定在25℃时的稳定性,为其贮存条件的选择提供依据。方法选择3个厂家3个批号的注射用头孢拉定样品在25℃下贮存3个月,依据《中国药典》2010年版二部注射用头孢拉定项下规定,考察其性状、溶液澄清度和颜色、水分、pH值、有关物质和含量的变化情况。结果注射用头孢拉定在25℃下贮存3个月,性状、水分、pH值、有关物质和含量均符合《中国药典》2010年版的规定;其中,一个厂家一个批次的样品溶液颜色在放置2个月后,颜色超过规定的黄绿色8号标准比色液。结论不同厂家生产的注射用头孢拉定其稳定性不同,大部分厂家的药品可在25℃下贮存3个月。     

仪器法测定药品颜色的研究

本文根据色度学原理,采用"L*a*b*均匀色空间"表色系统,用国产色差计对中国药典1990年版中黄色、黄绿色标准比色液和卡那霉素原料及其制剂5个品种共149批供试品的颜色进行了反复测量、分析。结果表明:不仅颜色的确定、表述有了精确的量值;而且仪器法测得各色调色号的色差等9个颜色参数与色号浓度相关性良好;重现性良好;标准比色液与水的色差值与水的色值可作为一个常数来使用;对比仪器法与目视法对供试品测色的结果,二者完全全吻合;并且仪器法显示出特殊的优越性:可克服目视法由于观察者的视觉差异、心理因素不同带来的主观误差;以及有时由于标准和供试品色调不符使得结果难以判断的缺点;特別是用目视法难以下结论的边缘产品,改用仪器法后,有具体的色差量值限度标准,结果极易判断。总之,仪器法测色可量化,精确,简便易行。本研究结果为中国药典收载仪器法测药品颜色提供了依据。     

诺氟沙星葡萄糖注射液的颜色控制

诺氟沙星葡萄糖注射液的颜色控制倪仕敏（湖南零陵地区药检所４２５０００）周玉泉（零陵地区卷烟厂职工医院）我们在考察诺氟沙星葡萄糖注射液（ＩＮＦＧ）质量时，发现有些产品按卫生部部颁标准检查，溶液的颜色不符合规定（规定：“本品与黄绿色４号标准比色液比较不得...     

利用溶液色差值与吸光度的相关性建立头孢西丁钠溶液颜色的仪器测定方法

目的 建立一种客观量化的注射用头孢西丁钠溶液颜色的仪器测定方法。方法 借助色差计考察色差值与溶液吸光度的相关性，选择相关性最强的波长作为检测波长，并在该波长下对注射用头孢西丁钠溶液颜色的药典标准进行限度转换。结果建立了在420 nm波长处测定注射用头孢西丁钠吸光度的溶液颜色仪器测定方法，吸光度限度规定为不得过0.17。结论 该方法能够准确量化测定并表述注射用头孢西丁钠的溶液颜色，为更好的研究与控制药品质量提供了数据支持，也为其他药品的溶液颜色检查从粗略的目视法转变为精准量化的仪器法提供了参考。     

Properties of colour reference solutions of the European Pharmacopoea in CIE L*a*b* colour space

The coordinates of CIE L*a*b* uniform colour space have been acquired from the transmitance spectra of colour reference solutions of European Pharmacopoeia (Ph.Eur.). Calculation of colour differences of these solutions from purified water deltaE* gave their values in the range between 0.7 (B9 solution) to 36 (Y1 solution) CIE units. Excluding red colour reference soulutions, deltaE* values did not depend on concentrations of colour compounds linearly. Small deltaE* values founded by the brown and brownish-yellow colour reference solutions of the lowest concentrations can possibly cause some problems of visual examination of the degree of coloration of liquids according to Ph.Eur.     

依米丁的比色测定法——次氯酸钠法

依米丁的含量測定,文献記載有容量法、重量法、非水溶液滴定法、螢光分析法、比色法等。药典一般采用容量法,卽以有机溶媒提取生物碱后,再用酸碱滴定的方法。但依米丁在加热或遇光时极易变貭而成去氫依米丁(dehydroemetine),往往影响結果的准确性。为了避免加热,有的药典用过量的酸来提取醚层中的生物碱,然后用碱滴定剩余的酸。关于比色法,Allport等建議用过氧化氫法;Rojahn等报告用苦味酸     

THE CONTRACTILE RESPONSE OF SMOOTH MUSCLE TO IMMERSION IN HYPERTONIC SOLUTIONS

1. Strips of bovine tracheal muscle and rabbit aorta produced sustained contractions on perfusion with Krebs solution made twice normal strength by addition of sucrose. The contractures were relaxed on return to normal Krebs solution. 2. Similar contractures were produced by tracheal muscle strips in Krebs solutions made twice normal strength by addition of galactose, glucose or NaCl whereas urea caused only a transient contraction. 3. In twice normal strength Krebs solution (sucrose added) the basal tension of rat portal vein and guinea-pig taenia coli was increased. Spontaneous mechanical activity was maintained, but the frequency of contractions was reduced. 4. The hypertonic contracture of bovine trachea in twice normal strength Krebs solution (sucrose added) was reduced by 15% by omission of Ca from the bathing fluid (01 mmol/1 EGTA added). Severe Ca depeletion, by prolonged washing in Ca-free Krebs with 12.5 mmol/1 EGTA and Carbachol added, resulted in a 77% reduction in the hypertonic contracture. 5. In twice normal Krebs solution (sucrose added), the hypertonic contracture was partially relaxed by isoprenaline (4 × 10^?6 mol/1); the contractile response to carbachol was reduced; the contractile response to high-K Krebs solution was maintained. 6. Atropine (5 × 10^?7 mol/1) abolished the contractile response to carbachol, but had no effect on the hypertonic contracture. 7. It is suggested that the contraction of bovine tracheal strips in hypertonic solutions is mainly due to activation of the contractile myofilaments rather than simple cell shrinkage. Hypertonic solutions may also interfere with some steps in the excitation-contraction coupling sequence.     

Ciprofloxacin determination by visible light spectrophotometry using iron(III)nitrate

A simple, rapid, efficient and inexpensive method was developed for the determination of ciprofloxacin in tablets and in solutions for infusion by visible light spectrophotometry using 1% iron(III)nitrate in 1% nitric acid. The complex formed by the iron(III)nitrate solutions and the sample and standard ciprofloxacin solutions gave origin to a compound of yellow-orange colour with maximum absorption at 435 nm, which was stable for 60 min. The Lambert-Beer law was obeyed in the concentration range of 20–100 μg/ml. The spectrophotometric method proposed for the evaluation of ciprofloxacin as a raw material and in tablets and solution for infusion is a good alternative method to that recommended by USP XXIII.     

偏最小二乘回归及其在消尔疴口服液紫外分光光度分析中的应用

偏最小二乘法在对因变量矩阵分解的同时,也依据主成分分析法将自变量矩阵分解,充分利用了两者的信息及内在联系,所得回归模型稳定性好,预示能力强。应用于消尔疴口服液的紫外分光光度分析中,同时测定了两主要成分磺胺噻唑和磺胺二甲嘧啶的含量,平均回收率分别为99.8%和100.4%,变异系数0.52%和0,60%,结果满意。     

ON THE REACTIVITY OF CARBOXYL GROUPS OF RIBONUCLEASE-A IN ANHYDROUS METHANOL

The esterification of Ribonuclease-A in methanol/0.1 M hydrochloric acid has been studied by measuring the decrease in the number of titratable groups of the protein and estimating the amount of methanol incorporated. Esterification of nearly five of the 11 free carboxyl groups of the protein resulted in almost complete inactivation of the enzyme. The initial products of esterification have been chromatographed on Amberlite columns, and five partially active methyl ester derivatives of Ribonuclease-A have been isolated. The dimethyl ester, the initial product of esterification with reduced catalytic activity, has the carboxyl groups of Glu-49 and Asp-53 modified. Even in the non-aqueous solvent, as in the native structure of the protein in aqueous solution, these carboxyl groups are the fast reacting ones. Subsequently, the esterification reaction appears to proceed preferentially at the C-terminal region of the molecule. Comparison of the reactivities of carboxyl groups of Ribonuclease-A in acidic methanol to that known in aqueous solutions (with carbodiimides) suggests that the structure of Ribonuclease-A in the non-aqueous solvent resembles, at least in part, the structure in aqueous environment.     

包公藤甲素两种缩瞳剂的生物利用度比较

本文报告用药理指标测定了两种包公藤甲素缩瞳剂的相对生物利用度。兔瞳孔直径的变化选作为分级定量的药理效应强度指标。观察的药理效应强度通过剂量-效应曲线,转换成相应的生物相药物浓度。然后,通过药一时曲线下面积计算包公藤甲素两种缩瞳剂的相对生物利用度。结果表明,用磷酸缓冲液(pH7)配制的缩瞳剂与用氯化钠调整渗透压配制的缩瞳剂(pH6)相比,其相对生物利用度为60%(P<0.05)。     

THE HAEM-ACCESSIBILITY IN LEGHAEMOGLOBIN OF LUPINUS LUTEUS AS OBSERVED BY PROTON MAGNETIC RELAXATION

Using the solvent-protons' longitudinal magnetic relaxation rates (p.m.r.) for Lupinus luteus leghaemoglobin derivatives the accessibility of the haem has been evaluated by our “stereo-chemical p.m.r. titration” method with nonexchangeable protons of aliphatic lower alcohols in otherwise deuterated solutions. The haem in leghaemoglobin is more accessible and its protein environment more flexible compared with vertebrate haemoglobins. The correlation time in aquometleghaemoglobin aqueous solution has been determined by measuring the frequency dispersion of the p.m.r. rates between 6.1 and 93 MHz. Taking into account the measured value of τ_c = (7.7 ± 0.5) × 10^-10 s the iron-to-proton inter-spin distances have been calculated. The significance of these distances as well as the electronic g-factor anisotropy for elucidation of fine structural details of the haem-environment are discussed.     

盐酸戊乙奎宁在水溶液中的降解机理

Penequine hydrochloride (Ⅰ) is a new potent anticholinergic drug, the degradation mechanism of Ⅰ in aqueous solutions is reported in this paper. Ⅰ is an ethereal compound, stable in neutral and alkaline solutions, but it decomposes in strong acidic solutions. Its main degradation products have been separated and identified by means of TLC, MS, GC/MS and GC/FTIR. With reference to the general degradation rule of ethereal compound and the structure of the degradation products, we deduced that the ether linkage of Ⅰ splits in acidic solutions by the catalysis of hydrogen ion, producing 3- quinuclidinol (DP1) and 1-phenyl- 1-cyclopentyl glycol. The latter turns into 1-phenyl-l-cyclopentyl acetaldehyde through dehydration and rearrangement. In addition, small amounts of other degradation compounds, e. g. benzaldehyde, acetophenone, phenylcyclopentyl ketone, etc. have also been found, but the mechanism remains to be further studied.