Fluorimetric assay of rufloxacin in serum and in pharmaceutical formulations

A simple and rapid fluorimetric method for the determination of 9-fluoro-10-[N-(4′-methyl)piperazinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-d,e][1–4]benzothyazin-6-carboxylic acid hydrochloride (MF 934), in serum and in pharmaceutical formulations, has been developed based on its strong fluorescence, in 0.1 N H₂SO₄, at 526 nm (excitation wavelength at 340 nm). The procedure which involves the direct dilution of the sample requires only a few minutes and the sample volume is only 20–100 μl of serum, depending on the drug concentration. Tedious sample preparation procedures such as extraction, deproteinization, or centrifugation are not necessary. The minimum concentration that can be detected is 0.3 ng ml⁻¹, the standard curve in 0.1 N H₂SO₄ was found to be linear from 0.005 to 1.5 μg ml⁻¹ and from 0.01 to 0.07 g in plasma after dilution with 0.1 N H₂SO₄.     

灵芝菌合剂中灵芝多糖含量的测定

目的：探讨灵芝菌合剂中灵芝多糖含量的检测方法。方法：采用分光光度法，以无水葡萄糖为对照品，检测波长为490nm。结果：此方法在0～120μg范围内线性关系良好，灵芝多糖的平均回收率为99．09%。RSB为1．14％。结论：本法简便快捷，准确度高，重现性好，可作为本制剂的质控方法。     

多层螺旋CT肺密度测定对结缔组织病肺问质病变的早期诊断

目的探讨多层螺旋CT(MSCT)肺密度测定对结缔组织病(CTD)肺间质病变(ILL)早期诊断的临床意义。方法对222例CTD患者及50名正常对照者，应用MSCT附带的Pulmo自动评估软件进行上、中、下肺区的密度测定，并同时进行肺高分辨扫描(}-IR(_1、)，分析二者的变化与CTD伴ILL的关系。结果222例cm患者中197例平均肺密度有不同程度的增高，25例平均肺密度正常。157例HRCT有不同程度的肺间质病变，65例HRCT正常。50名正常对照者HRCT均正常，8名平均肺密度有不同程度的增高，42名平均肺密度正常。结论采用MSCT与HRCT对CTD伴ILL的检测结果差异有统计学意义，P=0．000(双侧)，因此MSCT平均肺密度测定对早期诊断CTD伴ILL比HRCT更敏感，更有临床意义。     

蛋黄磷脂中磷脂酰乙醇胺的薄层扫描测定

将超临界ＣＯ２萃取法得到的蛋黄粉中的磷脂经薄层色谱分离，采用双波长薄层扫描仪对其磷脂酰乙醇胺进行测定。平均回收率为９７．６７％，ＲＳＤ为２．３１％。     

甘草黄酮的提取分离和含量测定

目的：充分利用甘草资源。方法：从提取过甘草酸的废渣中提取甘草黄酮并进行含量测定。结果：用碱酸处理和用大孔树脂处理黄酮含量高，收率也高。结论：从甘草废渣中提取甘草黄酮具有较好的社会效益和经济效益     

青霉素酶电极的研制

探讨了青霉素酶电极的制备方法，以青霉素酶为敏感膜偶合玻璃电极制成青霉素酶电极，在０．１５￣１．５ｍ ｍｏｌ／Ｌ青霉素钠浓度范围内，该电极的动力学响应与青霉素钠浓度的对数呈良好的线性关系，相关系数为０．９９８８，对电极性能的影响因素如介质条件，温度、膜厚度等进行了考察，并试验了电极的有效活性期。测得平均回收率为９９．０％。     

差示分光光度法测定伤风止咳露中盐酸异丙嗪的含量

采用差示分光光度法测定伤风止咳露中盐酸异丙嗪的含量。以Ｈ２Ｏ２冰醋酸为氧化剂将盐酸异丙嗪氧化，测定氧化前后的吸收度差值。其△Ａ值与盐酸异丙嗪在一定浓度范围内呈线性关系。该法操作简便、快速、结果准确。     

Capillary gas chromatographic assay of camphor and m-cresol in dermatological creams

Camphor and m-cresol mixtures are used in antiseptic and anti-itching creams. No compendial method exists for these preparations. This paper reports a capillary gas chromatographic method using FID detection with 2,6-di-tert-butyl-4-methylphenol as internal standard on a 30 m×0.32 mm Supelcowax®-10 column (0.25 μm film) with helium as carrier gas. Ramped temperature programming was applied. The method allows simultaneous quantitation of camphor and m-cresol in the presence of o- and p-cresols, calamine and zinc oxide. Overall percent recoveries (±SD, n=9) of camphor, o-, p- and m-cresol from spiked placebo creams, at a labeled amount of 10 (w/w)% were 96.9±0.6, 98.2±0.6, 99.2±0.5 and 101.0±0.9%, respectively, and at a labeled amount of 1% were 96.7±0.6, 97.8±0.9, 97.8±0.6, and 100.3±1.0%, respectively. The recovery studies were carried out at ±30% of the labeled amounts. Linear peak area or height ratios were obtained (r>0.999) for camphor, o-, p- and m-cresol covering a concentration range of 10–200% of the labeled amount. Linearity (r>0.999) was also obtained for m-cresol when the relative concentration of o- and p-cresol was varied from 5 to 100% of the m-cresol concentration. The resolution between the ‘critical pair’ of p- and m-cresol was ≥1.1. The limit of quantitation was 23 pg for m-cresol and 9.3 pg for camphor using an injection split of 1:50. The repeatability (%RSD) for all compounds were <2% for peak area and <1.4% for peak height ratios. System suitability and robustness of the method were established. The method was successively applied to the assay of available commercial products and allows assay of camphor and the three cresol isomers.     

复方栀子冲剂栀子甙薄层扫描测定

应用薄层扫描法测定了复方栀子冲剂中栀子甙的含量，对实验条件，以正交试验法进行优选，确定了最佳方案，排除了干扰，得到了满意的效果。