荧光分光光度法测定复方制剂中的盐酸普鲁卡因

本文用荧光分光光度法不经分离直接测定复方制剂中盐酸普鲁卡因的含量。其最大激发波长及最大发射波长分别为２９０．０ｎｍ，３５６．０ｎｍ。标准曲线浓度范围为０．６～１．４μｍ／ｍｌ，回归方程为Ｙ＝４８．８４１７Ｘ＋６．３０５（ｎ＝６），ｒ＝０．９９９８，４种样品平均回收率为９９．９５％（ｎ＝６），ＲＳＤ＝０．４７％。     

高效液相色谱法测定人及兔血浆或血清中α—生育酚

本文介绍用反相高效液相色谱法测定人及兔血浆或血清中α－生育酚，血样用乙醇沉淀蛋白，正己烷溶剂提取后，以Ｃ８化学键合硅胶为固定相，甲醇－水（９６：４，ｖ／ｖ）为流动相，醋酸α－生育酚为内标，在２８５ｎｍ波长定量检测。在１～３０μｇ／ｍｌ波度范围内线性关系良好，最低检测限为０．１μｇ／ｍｌ。对血浆样品的日间（ｎ＝６）及日内（ｎ＝８）测定变异系数分别小于４．２％和１，７％。检测血浆中α－生育酚的回收率为９１．５～１０３．８％。应用本法测定正常人血清中α－生育酚浓度为１２．６７，±３．２μｇ／ｍｌ（ｎ＝２７），并测定观察了兔口服维生素Ｅ后不同时间血浆中浓度变化情况。     

反相高效液相色谱法测定阿霉素的血药浓度

本文采用反相ＨＰＬＣ法测定阿霉素的血药浓度，血浆样品用甲醇－氯仿（１：４）在ｐＨ９．０的条件下提取后进样，５ｍｍｏｌ／Ｌ磷酸－异丙醇－甲醇－乙腈（４５：３５：１０：１０，ｐＨ２．９）为流动相，荧光检测器λｅｘ＝４５０ｎｍ，λｅｍ＝５３０ｎｍ。最低检测浓度１０ｎｇ／ｍｌ，线性范围在３０－１５００ｎｇ／ｍｌ内ｒ＝０。９９８７，日内ＲＳＤ为１．５％－２．４％，日间ＲＳＤ为１．８％－３．７％。并对７例肺癌     

柱切换HPLC法测定人血浆中阿霉素浓度

本文采用ＨＰＬＣ柱切换技术建立了阿霉素（Ａｄｒｉａｍｉｃｉｎ）血药浓度的测定方法。以μ－ＢｏｎｄａｐａｋＣ_（１８）（３７～５０μｍ）为预处理柱（５０ｍｍ×５ｍｍＩＤ），磷酸缓冲液为预处理流动相，对样品进行自动净化处理。分析柱（１５０ｍｍ×５ｍｍＩＤ）固定相为ＹＷＧ－Ｃ１８，１０μｍ，流动相为甲醇－乙腈－磷酸缓冲液（４０：１０：５０，Ｖ／Ｖ）的混合溶液。荧光检测波长为λ_（ｅｘ）＝４９５ｎｍ，λ_（ｅｍ）＝５６０ｎｍ。血浆测定的线性范围为３～６８２ｎｇ／ｍｌ，ｒ＝０．９９９８，血浆中最低检测浓度为１ｎｇ／ｍｌ。方法的平均回收率为１０１．０％，日内及日间相对标准偏差均小于６％。     

荧光光谱法测定硫酸庆大霉素注射液的含量

本文报告了以乙酰丙酮、甲醛为荧光衍生试剂，建立了测定硫酸庆大霉素注射液含量的荧光光谱法。激发波长４２２ｎｍ，荧光波长４８２ｎｍ。硫酸庆大霉素浓度在０～６ＩＵ／ｍｌ范围内与荧光强度成线性关系（ｒ＝０．９９９７），平均回收率为１０１．１～１０２．０％，ＲＳＤ在１．５％以下。本法操作简便、灵敏，试剂价廉易得，适用于硫酸庆大霉素注射液的含量测定。     

紫外分光光度法测定利福平的血药浓度

作者采用紫外分光光度法测定人血浆中利福平的浓度。血浆样品用乙酸乙酯提取，测定波长为３３８ｎｍ其平均回收率为９６．７２％，ＲＳＤ为１．４６％。实验表明：利福平浓度在２～１２μｇ／ｍｌ范围内线性关系良好（ｒ＝０．９９９４）。口服利福平０．４５～０．６０ｇ后９ｈ，测得血药浓度在１．３０～７．９３μｇ／ｍｌ之间，本文方法简单、快速，结果令人满意。     

HPLC测定血浆中奥美拉唑的浓度

本文采用ＨＰＬＣ测定人血浆中奥美拉唑的浓度、色谱柱为ＵｌｔｒａｓｐｈｅｒｅＯＤＳ４．６×２５０ｍｍ，流动相为甲醇－磷酸盐缓冲液（６０／４０），检测波长为３０２ｎｍ，流速为１ｍｌ／ｍｉｎ，血浆浓度在０．０２５～１．０μｇ／ｍｌ范围内线性关系良好（γ＝０．９９９８），最低检测浓度０．０２５μｇ／ｍｌ，平均回收率１００．５±１．９％。日间、日内ＲＳＤ％均＜４．１％。     

高效液相色谱法测定痛特灵霜中双氯芬酸的含量

本文采用ＨＰＬＣ法，建立了痛特灵霜中双氯芬酸的含量测定方法。用地塞米松为内标，样品加超纯水超声振荡提取后，用０．４５μｍ滤膜滤过，进样１０μｌ，采用国产ＹＷＧ－Ｃ＿（１８）柱分离，甲醇：水：醋酸（８０：２０：２）的混合溶液为流动相，２７５ｎｍ波长处检测。样品保留时间为４．６３ｍｉｎ。标准曲线浓度在０．５～４０μｇ／ｍｌ范围内线性关系良好（ｒ＝０．９９９９）。最低检测浓度为０．１２５μｇ／ｍｌ。方法的绝对回收率平均为９８％（ｎ＝６），ＲＳＤ为１．８％。相对回收率平均为９９．８％（ｎ＝６），ＲＳＤ＝１．０％。日内ＲＳＤ为０．５％～１．８％，日间ＲＳＤ为０．８％～６．５％。测定三批样品，平均百分含量为９７．９９％。     

反相高效液相色谱法测定格列甲嗪血浆浓度

应用反相高效液相色谱法测定格列甲嗪血浆浓度。色谱柱为ＯＤＳＣ１８柱，流动相为乙腈─甲醇─水（４０：２０：４０Ｖ／Ｖ），内含０．１％冰醋酸和０．０８％三乙胺。流速０．５ｍｌ／ｍｉｎ，柱温５０℃，检测波长２７５ｎｍ。线性范围在０．０２～１．００μｇ／ｍｌ（ｒ＝０．９９９９）。检测下限为０．０１μｇ／ｍｌ。平均回收率为９９．０±２．８％，ＲＳＤ＝２．８２％。日内及日间测定相对标准偏差均小于５％。     

反相高效液相色谱法测定大蒜素的血药浓度

目的：建立反相高效液相色谱法测定血清中大蒜素的浓度。方法：血清样品用１０％三氯醋酸沉淀蛋白,正己烷提取后进样。采用Ｐｈｅｎｏｍｅｎｅｘ Ｃ１８（２５０ｍｍ × ４．６ｍｍ,５μｍ）柱;流动相：乙腈－１％冰醋酸（６２：３８,Ｖ／Ｖ）,ｐＨ＝３．５;流速：１．２ｍｌ／ｍｉｎ,在室温下;波长：２４０ｎｍ检测。结果：该方法回收率为（９９．２±６．６）％,最低检测浓度为０．１８μｇ／ｍｌ,大蒜素血药浓度在０．２９～１２．４μｇ／ｍｌ范围内峰面积与浓度线性关系良好（ｒ＝０．９ ９７７）,日内 ＲＳＤ＜５．５％（ｎ＝５）,日间 ＲＳＤ＜５．８％（ｎ＝５） 结论：本法快速、准确、灵敏,能较好满足大蒜素临床药代动力学研究的需要。     

Biphasic effect of a kappa-opioid receptor agonist on plasma oxytocin levels in rats

The effect of the kappa-opioid receptor agonist, bremazocine, on plasma oxytocin levels in rats was measured by a sensitive radioimmunoassay. Initially, a decrease in plasma oxytocin levels was seen 30 min after injection. This was in accordance with the bremazocine inhibition of oxytocin release after submaximal electrical stimulation seen in isolated neurointermediate lobes. The initial decrease in plasma oxytocin reversed, and 4 h after injection of bremazocine a 20-fold increase in the oxytocin level was seen. The rise in plasma oxytocin was paralleled by a rise in plasma sodium. The biphasic time course of the plasma oxytocin response can be explained by a combination of an inhibition of oxytocin release from the neurohypophysis and an increased water excretion leading to an elevation in plasma sodium, which may be responsible for the late rise in plasma oxytocin. Down-regulation of the opioid receptors may also contribute to the delayed rise in plasma oxytocin.     

男性不育症患者精浆酸性磷酸酶对精浆生化指标的影响

目的研究男性不育症患者精浆酸性磷酸酶对精浆生化指标的影响。方法以539例男性不育症患者为研究对象,根据精浆酸性磷酸酶水平分为观察组和对照组,精浆酸性磷酸酶〉48．8U／mL为正常组,〈48．8U／mL为对照组,对两组患者精浆生化指标进行比较分析,通过相关性分析比较539例患者精浆酸性磷酸酶与精浆生化指标的相关性。结果观察组精浆锌明显低于对照组,精浆弹性蛋白酶明显高于对照组,曲组相比差异有统计学意义（P〈0．05）,精浆酸性磷酸酶与精浆锌的相关系数为0．612,呈明显正相关（P〈0．05）,与精浆弹性蛋白酶的相关系数为-0．325,呈明显负相关,而与精浆α-糖甘酶及果糖无相关性（P〉0．05）．结论联合检测精浆酸性磷酸酶、锌及弹性蛋白酶对于前列腺相关炎性疾病的诊断及治疗疗效的判定有重要的临床应用价值。     

Factors affecting the free plasma fraction of phenytoin in patients with epilepsy

The variability and possible factors modifying the free plasma fraction of phenytoin were investigated in 134 patients with epilepsy undergoing long-term treatment. The total and free plasma concentrations of phenytoin were determined using fluorescent polarisation immunoassay. Concentrations of albumin, bilirubin and creatinine were also obtained. The free plasma concentration was separated by ultrafiltration, at 25 degrees C, using Centrifree((R)) filters. Factors related to the free plasma fraction of phenytoin (free plasma concentration/total plasma concentration) were gender, age, dose, therapeutic regimen, total plasma concentration and the biochemical parameters mentioned. The mean of free plasma fraction was 9.1% with a very high variability (between 3.3 and 37%). No significant relationship was found between the free plasma fraction and dose, age, gender, total plasma concentration or the biochemical data. The only variable with a significant effect (p < 0.05) on the free plasma fraction was polytherapy with valproic acid. The variability in the free plasma fraction of phenytoin was high in epileptic patients, and was poorly related to the clinical or analytical variables studied. In the absence of pathologies that modify phenytoin binding (uraemia, hypoalbuminaemia), the only factor predictive of a possible alteration in the binding of phenytoin to plasma proteins was polytherapy with valproic acid.     

Differences in the binding of drugs to plasma proteins from newborn and adult man. I

Summary The binding of various drugs to plasma proteins from adult and cord plasma was determined by equilibrium dialysis. For almost all the drugs binding to cord plasma was lower than to plasma from adults. No evidence was found that the difference in binding was due to the different protein concentration in cord and adult plasma or to an influence of substances in ultrafiltrates of the plasmas.     

血浆中细菌内毒素定量测定方法的研究

目的:建立定量测定血浆中细菌内毒素的实验方法。方法:以内毒素检查用水制备标准曲线,动态浊度法定量测定分别采用3种抗凝剂的抗凝血中细菌内毒素的含量及回收率;以正常人血浆制备内毒素标准曲线,以抗增液复溶鲎试剂,动态浊度法定量测定人血浆中内毒素的含量及回收率。结果:使用肝素钠抗凝的血浆溶液对内毒素测定无干扰,而其他抗凝剂肝素锂、EDTA-K2等有干扰;人血浆经稀释加热处理,配合使用抗增液后制备的标准曲线与使用内毒素用水制备的标准曲线相比,可以更好地测定人血浆中细菌内毒素的含量,且具有较好的重现性;用所建立的方法测定肠癌患者血浆中内毒素的含量,其结果显著高于正常人血浆中内毒素的含量。结论:以肝素钠作抗凝剂,血浆经稀释加热处理并配合使用抗增液可定量测定血浆中细菌内毒素的含量。     

SALIVARY CONCENTRATIONS OF ATRAZINE REFLECT FREE ATRAZINE PLASMA LEVELS IN RATS

The protein binding of atrazine in plasma and its effect on salivary excretion of atrazine was determined in male Sprague-Dawley rats. The degree of protein binding of atrazine was determined at 3 steady-state plasma concentrations, 50, 150, and 250 mug/L, using an ultrafiltration technique. In total, 48 arterial blood samples were collected from 18 rats; 38 of 48 blood samples had their time-matched whole saliva samples. The average protein binding of atrazine ranged from 18% to 37% ; however, it was not significantly different across the 3 steady-state plasma concentrations nor among the individual rats. Overall, 26% of atrazine was bound to plasma proteins and not available for transport from blood into saliva. Protein binding of atrazine in plasma was not correlated with total atrazine plasma concentration nor with free atrazine plasma concentration, which indicates that the protein-bound fraction of atrazine is independent of plasma concentration within the range measured in this study (30-400 mug/ L). The average saliva/ plasma (S/P) concentration ratio of atrazine increased from 0.7 using total atrazine plasma concentration to 0.94 (S/fP) when free atrazine plasma concentrations calculated as 26% of protein binding was used. Salivary concentration was highly correlated with free atrazine plasma concentration. The results suggest that salivary concentration of atrazine not only reflects its total plasma level but accurately measures the portion of atrazine (free atrazine) in plasma, which may be of toxicological significance.     

Mesalazine release from a pH dependent formulation: effects of omeprazole and lactulose co-administration

Aims The plasma binding of the cyclosporin D analogue SDZ PSC 833 was investigated in vitro .
Methods The plasma total binding constant (corresponding to the bound-to-free concentration or binding ratio) was determined at 37°  C by the erythrocyte partitioning technique on plasma samples from three healthy volunteers and three cancer patients. Lipoproteins were also removed from plasma samples from three healthy volunteers by a standard ultracentrifugal technique.
Results SDZ PSC 833 plasma binding was 97.8±1.1% and 97.3±0.2% in samples from three healthy volunteers and three cancer patients respectively. More than 95% of blood SDZ PSC 833 was distributed in plasma. When the original plasma samples of three individuals were delipidated, SDZ PSC 833 binding was strongly decreased (58% bound to plasma proteins) and when lipoproteins were resuspended in the delipidated plasma samples to produce varying lipoprotein plasma concentrations, the binding increased continuously with the fraction of added lipoproteins. When lipoproteins were resuspended to restore the original lipoprotein plasma content, the % plasma-bound SDZ PSC 833 increased to 98.2%, close to the value observed with the original plasma (98.7%).
Conclusions These results clearly indicate that SDZ PSC 833 plasma binding is mainly determined by lipoproteins and that in blood, most of SDZ PSC 833 is distributed in plasma.     

Can fluconazole concentrations in saliva be used for therapeutic drug monitoring?

The saliva/plasma concentration ratio of fluconazole was investigated in 22 HIV-1-infected individuals with an oropharyngeal Candida infection to determine whether saliva fluconazole concentrations could provide useful information for therapeutic drug monitoring in this population. Steady-state paired plasma and saliva samples were obtained after approximately 1 week of treatment with 50-or 100-mg fluconazole as capsules. A significant correlation between plasma and salivary levels of fluconazole was observed. The median saliva/plasma concentration ratio was 1.3 and was independent of the ingested dose and the plasma fluconazole concentration. The prediction of fluconazole concentrations in plasma from the concentrations in saliva was, although unbiased, not precise. From these findings, the authors conclude that although stimulated salivary fluconazole concentrations are significantly correlated with plasma concentrations, it is not possible to predict plasma fluconazole levels from the salivary concentrations with adequate precision. However, saliva fluconazole concentrations have sufficient value to test for compliance and even semiquantitative prediction of plasma concentrations.     

超滤法结合液质联用技术测定抗肿瘤化合物CJ-6在不同种属中的血浆蛋白结合率

目的:通过建立测定血浆中抗肿瘤化合物N-(4-((2-(环丙烷甲酰胺)吡啶-4-基)氧基)-3-氟苯基)-4-甲基-3,5-二氧基-2-苯基-2,3,4,5-四氢-1,2,4-三嗪-6-甲酰胺(CJ-6)的分析方法,测定CJ-6在不同种属(大鼠、猴、人)中的血浆蛋白结合率.方法:采取超滤法测定CJ-6在大鼠、猴、人血浆...     

Effects of calcium antagonism on the resting and exercise-stimulated renin-aldosterone axis

The effect of short-term calcium antagonism with felodipine on blood pressure and on some biochemical plasma variables such as catecholamines, renin and aldosterone was studied in 10 normal volunteers at rest and during incremental bicycle exercise. At rest, diastolic blood pressure was slightly decreased during felodipine, whereas systolic pressure and heart rate were not significantly changed. The plasma noradrenaline concentration and plasma renin activity were increased during felodipine treatment; the plasma adrenaline and aldosterone concentrations on the contrary, were not significantly changed. The rises in plasma renin activity, plasma aldosterone and plasma adrenaline and noradrenaline concentrations produced by exercise were not significantly affected by felodipine. The plasma calcium concentration was significantly higher during felodipine treatment than during placebo and this was accompanied by an increased urinary calcium excretion. It is concluded that the rise in plasma renin activity during calcium antagonism with felodipine is not accompanied by a significant increase in plasma aldosterone. Furthermore, the present data suggest that, at least during exercise, calcium antagonism does not interfere with the mechanisms underlying the exercise-induced activation of renin and aldosterone release.