双香退热口服液GC指纹图谱分析及4种指标成分含量测定

目的 建立双香退热口服液指纹图谱方法,并同时进行4种指标成分含量测定。方法 采用HP-5弹性石英毛细管柱（30 m×0.32 mm,0.25 μm）;柱升温程序：起始温度110℃,保持10 min,25℃·min^-1的速度升温至230℃,保持9.2 min;进样口温度220℃;FID检测器温度220℃;载气：高纯N₂（>99.99%）;柱流量1.0 mL×min^-1;分流比10：1;进样量1 μL。结果 建立了双香退热口服液GC指纹图谱方法,10批成品中检测到的色谱峰为13个,其中1,2,3,4号峰来源于香薷药材,5,6,7,8号峰来源于厚朴药材,9~13号峰在香薷和厚朴药材及其阴性中均有出现,初步推测此类成分为香薷和厚朴两药材共有成分。以对照品与样品出峰时间比对,标定1号峰为麝香草酚、2号峰为香荆芥酚、7号峰为厚朴酚、8号峰为和厚朴酚,4种指标成分线性范围分别为0.226~2.260 mg·mL^-1,0.105 5~1.055 0 mg·mL^-1,0.082 8~0.828 0 mg·mL^-1,0.072 0~0.720 0 mg·mL^-1。平均加样回收率分别为100.1%~103.5%,100.2%~104.4%,99.4%~100.7%,96.3%~99.27%;RSD分别为2.8%,2.1%,2.4%,2.1%。结论 本法稳定、合理、可行,为该复方中药质量评价提供科学依据。     

仿生提取-高效液相色谱-电感耦合等离子体质谱技术测定冰硼散及朱砂药材中可溶性汞的含量

目的： 建立仿生提取-高效液相色谱-电感耦合等离子体质谱技术测定冰硼散及朱砂药材中可溶性汞含量的分析方法，可用于研究冰硼散及朱砂药材的用药安全性。方法： 通过模拟人体胃肠道环境，采用人工胃液提取冰硼散及朱砂中的可溶性汞，结合高效液相色谱（以十八烷基硅烷键合硅胶为填充剂；8%甲醇-0.06 mol·L^-1乙酸铵-0.05% 2-巯基乙醇的水溶液为流动相；流速0.4 mL·min^-1；进样体积20 μL）-电感耦合等离子体质谱技术进行分析测定。结果： 通过检测15批冰硼散样品及9批朱砂药材，结果甲基汞、乙基汞、无机汞分别在0.0007~0.28、0.007~1.4、0.17~34 ng·mL^-1范围内，浓度与峰面积呈良好的线性关系，r值分别为0.9997、0.9995、0.9998，平均回收率分别为96.8%、99.7%、98.0%，RSD分别为2.3%、2.8%、5.5%（n=6）。冰硼散中甲基汞含量为0.00046~0.018 mg·kg^-1，无机汞含量为0.64~4.73 mg·kg^-1，乙基汞含量为0.075~0.096 mg·kg^-1；朱砂中甲基汞含量为0~0.034 mg·kg^-1，无机汞含量为8.54~101.07 mg·kg^-1，乙基汞含量为0~0.82 mg·kg^-1。结论： 该方法简便、快速、灵敏，重现性好，可用于冰硼散及朱砂药材中可溶性汞的测定。     

HPLC测定盐酸达泊西汀片中的异构体

目的 建立盐酸达泊西汀片剂中异构体的HPLC检测方法。方法 采用DAICEL CHIRALPAK OZ-H色谱柱（250 mm×4.6 mm,5 μm）,柱温：40℃,检测波长：293 nm,流速：1.0 mL·min^-1,流动相：正己烷-异丙醇-二乙胺（80：20：0.05）。结果 盐酸达泊西汀及其异构体在0.01~0.50 mg·mL^-1内具有良好的线性关系（r=0.999 9）,盐酸达泊西汀定量限为0.002 mg·mL^-1（相当于0.02%）,最低检测限为0.001 mg·mL^-1（相当于0.01%）;异构体定量限浓度为0.001 mg·mL^-1（相当于0.01%）,最低检测限为0.000 5 mg·mL^-1（相当于0.005%）。结论 该方法操作简便,结果准确,可用于盐酸达泊西汀片剂中异构体的含量测定。     

GC法同时测定狗皮膏中樟脑、异龙脑、龙脑的含量

目的: 测定狗皮膏中樟脑、异龙脑及龙脑的含量。方法: 采用气相色谱法,以交联聚乙二醇为固定相的弹性石英毛细管柱,FID检测器。结果: 樟脑线性范围为0.182 1～9.104 0 mg·mL^-1,平均回收率102.2%(RSD为3.3%);异龙脑线性范围为0.031 4～1.570 0 mg·mL^-1,平均回收率101.7%(RSD为3.2%);龙脑线性范围为0.050 8～2.539 5 mg·mL^-1,平均回收率101.1%(RSD为3.4%)。结论: 本法简便、准确,可用于狗皮膏的质量控制。     

GC测定鱼肝油中EPA和DHA含量

目的 建立加校正因子GC内标法测定鱼肝油中EPA和DHA含量。方法 样品经皂化、甲酯化、异辛烷提取,采用DB-23（30 m×0.25 mm,0.25 μm）毛细管柱,FID检测器,程序升温（起始温度170℃,以1℃·min^-1的速率升温至225℃,保持5 min）,进样口温度为250℃,检测器温度为280℃,高纯N2为载气,流速为1.0 mL·min^-1,分流比为100∶1,二十三烷酸（C23∶0）甲酯为内标物。结果 EPA、DHA的峰面积比和浓度比分别在0.048 7~9.740 mg·mL^-1,0.051 0~10.206 mg·mL^-1内呈良好的线性关系（r=1.000 0）,EPA、DHA的平均回收率分别为98.7%（RSD=0.98%）,99.4%（RSD=1.34%）。结论 该方法简便、准确、重复性好,可用于鱼肝油的质量控制和掺假鉴定。     

HPLC测定人血浆中吡非尼酮浓度的不确定度评定

目的 建立HPLC测定人血浆中吡非尼酮浓度的不确定度分析方法。方法 分析HPLC测定吡非尼酮浓度的全过程,分析测量不确定度的来源和大小,量化各个测量不确定度分量,合成标准测量不确定度并报告扩展测量不确定度。结果 人血浆中低浓度（0.511 0 mg·mL^-1）、中浓度（2.038 mg·mL^-1）和高浓度（19.95 mg·mL^-1）的扩展不确定度分别为0.105 1,0.137 6,1.069 mg·mL^-1（P=95%）。结论 本方法不确定度来自标准曲线的拟合,其适用于HPLC测定人血浆吡非尼酮的不确定度评定。     

邻苯二甲醛柱前衍生化-HPLC测定复方氨基酸注射液中蛋氨酸亚砜的含量

目的 建立测定复方氨基酸注射液中蛋氨酸亚砜含量的方法。方法 采用邻苯二甲醛（O-phthaladehyde,OPA）柱前衍生HPLC。色谱柱为Agilent ZORBAX Eclipse AAA C₁₈柱（150 mm×4.6 mm,5µm）,检测波长为338 nm,流动相A为0.04 mol·L^-1磷酸二氢钠溶液（调节pH至7.8）,流动相B为乙腈-甲醇-水（45：45：10）,梯度洗脱,流速为2.0 ml·min^-1,柱温为40℃,供试品溶液与OPA衍生剂及硼酸盐缓冲液按设定程序自动混匀后进样。结果 蛋氨酸亚砜的质量浓度线性范围为0.000 5~0.050 0 mg·mL^-1（R=0.999 9）;定量限为0.250 5 μg·mL^-1,检测限为0.083 5 μg·mL^-1;精密度、稳定性、重复性试验的RSD<3.0%;平均回收率为99.1%（RSD=1.33%,n=9）。结论 该方法操作简便,可用于复方氨基酸注射液中蛋氨酸亚砜的含量测定。     

HPLC-CAD测定羟基脲胶囊含量及有关物质

目的 建立测定羟基脲胶囊含量及有关物质检查的HPLC-CAD方法。方法 采用Phenomenx Luna^® NH₂柱（250 mm×4.6 mm，10 μm，100Ǻ），柱温为40℃；以乙腈-水（82：18）为流动相，流速为1.0 mL·min^-1，检测器为电雾式检测器，雾化温度50℃，进样量10 μL。结果 在选定的色谱条件下，主峰与各杂质峰均能良好分离。采用外标法计算羟基脲胶囊的含量，采用主成分自身对照法计算脲的含量；羟基脲和脲分别在0.304 8~1.270 0 mg·mL^-1（r=0.999 8）、0.241 1~1.004 6 mg·mL^-1（r=1.000 0）内与峰面积呈良好线性关系。脲的检测限和定量限分别为2.82 ng和8.46 ng。结论 本方法操作简便，专属性强，结果可靠，可用于羟基脲胶囊的含量及有关物质的测定。     

金荞麦提取物体外抗流感病毒作用研究

目的 研究金荞麦提取物的体外抗流感病毒作用。方法 采用血凝试验,考察金荞麦提取物对鸡胚内流感病毒增殖的抑制作用;采用MTT法检测细胞活性,考察金荞麦提取物对流感感染细胞活性的影响。结果 与病毒对照组比较,金荞麦提取物高剂量组（10 mg·mL^-1）、中剂量组（5 mg·mL^-1）均能显著降低鸡胚尿囊液的血凝滴度（P<0.01）,而低剂量组（2.5 mg·mL^-1）则无显著性差异;在0.63~2.50 mg·mL^-1浓度内,金荞麦提取物各剂量组流感感染细胞的活性均明显高于病毒对照组,组间均存在显著性差异（P<0.01）,且病毒抑制率随着药物浓度的增大而增高,呈一定的量效关系,其中金荞麦提取物最大无毒浓度（2.5 mg·mL^-1）对流感病毒的直接抑制率达66.12%。结论 金荞麦提取物具有一定的体外抗流感病毒作用。     

柱前衍生-HPLC测定白消安在家兔体内的药动学参数

目的 建立测定家兔血清中白消安浓度和家兔体内药动学特征的柱前衍生化HPLC。方法 以1,5-戊二醇二甲磺酸酯为内标,二乙基二硫代氨基甲酸钠为衍生化试剂。流动相：甲醇-水（54∶46）,流速：0~20 min（1.0 mL·min^-1）,20~27 min（1.3 mL·min^-1）。柱温：30℃,检测波长：280 nm,进样量：25 μL。家兔分别以灌胃、静注的方式给予白消安,按本法测定血药浓度,DAS 3.0计算药动学参数。结果 白消安的血药浓度在0.1~3.4 mg·-L¹ 内线性关系良好（r=0.999 7）,日内、日间精密度以及样品稳定性符合中国药典2015年版的规定。低、中、高浓度的萃取回收率分别为90.0%,89.0%,91.5%。不同给药途径获得的药动学参数：单剂量口服t_1/2=（2.26±0.66）h,k=（0.33±0.12）·h^-1,k_a=（2.54±1.3）·h^-1,AUC_0–t=（1.95±0.18）h·mg·mL^-1;单剂量静脉注射t_1/2=（1.53±0.09）h,k=（0.45±0.03）·h^-1,AUC_0–∞=（4.38±0.26）h·mg·mL^-1。多剂量口服后C_ss=（0.48±0.03）mg·mL^-1,AUC_0–τ=（3.87±0.26）h·mg·mL^-1。结论 建立的柱前衍生-HPLC法适用于白消安血药浓度测定及药动学研究,不同给药途径的药动学参数为临床药动学研究提供了依据。     

Deamination of beta-phenylethylamine by monoamine oxidase--inhibition by imipramine

The oxidative deamination of tyramine (Tyr), 5-hydroxytryptamine (5-HT), and β-phenylethylamine (PEA) by mitochondrial preparations of rabbit lung and brain was inhibited by imipramine. This tricyclic iminodibenzyl antidepressant drug was most effective in decreasing the deamination of PEA: at 1 × 10^?4M imipramine, deamination of PEA, Tyr and 5-HT was inhibited by approximately 70, 45 and 45 per cent, respectively, when either lung or brain mitochondrial monoamine oxidase (MAO) preparations were used. Imipramine-induced inhibition of MAO was shown to be of a mixed type based on Lineweaver-Burk plots, but was found to be completely reversible. The desmcthyl and didesmethyl derivatives of imipramine were equally as effective as the parent drug in inhibiting the deamination of PEA, whereas the N-oxide analog of imipramine was less effective as an inhibitor of this reaction. These results support the premise that the action of imipramine as a clinically effective antidepressive agent may be related to its inhibitory effect on the specific form of MAO which deaminates PEA.     

Augmentation by serrapeptase of tissue permeation by cefotiam

Cefotiam (CTM) is a new cephalosporin with a broad spectrum of activity against both Gram-positive and Gram-negative microorganisms. Cephalosporins are widely used for prophylaxis of infections in patients undergoing thoracotomy. Augmentation by serrapeptase on tissue permeation of CTM was examined in 35 thoracotomy patients with lung cancer. The subjects were divided into two groups according to the method of the administration of CTM. Group I consisted of 17 subjects, each of whom received a single dose of 2 g of CTM alone by an instillation for 30 minutes. Group II consisted of 18 subjects, each of whom received a combination of CTM and serrapeptase; serrapeptase was given 2 tablets (10 mg) each time for three times/day until the day before surgery, and then CTM was administered by the same procedure. The following results were obtained: Individual difference was observed for the permeation of CTM into tissues. Pathologic differences also affected the permeation. Nevertheless, the CTM levels in pulmonary tissues reached about a half of those in the blood in both the single dose group and the combination group, hence sufficient concentrations exceeding MIC80 for main microorganisms that caused infections in the lung were obtained. The concentrations of CTM in inflammatory tissues have showed lower levels than those of normal tissues in both CTM single dose and the combination groups. Decrease of blood flow volume may have contributed to the reduction in levels of CTM in the inflammatory tissues. The ratio of the concentration of the drug in pulmonary tissues to that in the blood was 29.1 +/- 2.5% in the single dose group, and 44.2 +/- 6.0% in the combination group, the latter showing quite a significant increase (P less than 0.05). Combined administrations of CTM and serrapeptase deserves more trials in the case when surgical treatments of the lung are performed. An antiinflammatory effect of serrapeptase in the respiratory system is expected, and in addition, the combined use of CTM and serrapeptase should stimulate permeation of the antibiotic into tissues.     

Antagonism of morphine by beta-melanocyte-stimulating hormone and by tetracosactin

Using the decerebrate—spinal Lloyd preparation morphine depressed evoked mono- and polysynaptic reflex activity, β-melanocyte-stimulating hormone enhanced monosynaptic reflex activity, and tetracosactin had no effect. When morphine injection was preceded either by β-melanocyte-stimulating hormone or by tetracosactin a statistically significant depression was not observed. The stimulant actions of β-melanocyte-stimulating hormone did not appear to account for its capacity to antagonize morphine. The fall of blood pressure which follows the administration of morphine in this preparation was not antagonized by the prior administration of either polypeptide.     

Analgesia induced by brief footshock is inhibited by 5-hydroxytryptamine but unaffected by antagonists of 5-hydroxytryptamine or by naloxone

Exposure to footshock (1 mA) for 30 sec induced a marked analgesia that was enhanced by pretreatment with the 5HT synthesis inhibitor, p-chlorophenylalanine, and attenuated by the 5HT releasing drugs p-chloroamphetamine and fenfluramine, by the 5HT re-uptake inhibitor, fluoxetine and by the 5HT agonists, 5-methoxy-N,N-dimethyltryptamine and MK212. However, agonists, quipazine and trifluoromethylphenylpiperazine, with greated reported affinities for 5HT binding sites on rat brain membranes than MK212 were without effect as were the antagonists metergoline, methysergide, cyproheptadine, mianserine and methiothepin. The specific opioid antagonist naloxone was also without effect. The results in general indicate that analgesia induced by brief footshock (1 mA, 30 sec) is inversely related to 5HT availability but thereis little evidence of involvement of known 5HT receptors.     

Synergism by caffeine and by cocaine of the motor control deficit produced by midazolam

To evaluate the effects of caffeine and cocaine on the impairment of discriminative motor control produced by midazolam, rats were trained to hold a force transducer operated with a paw so that it remained between upper and lower limits of a force band for a continuous 1.5-s period to deliver each food pellet. Acute doses of 3 mg/kg midazolam SC impaired motor performance. Except for one animal, caffeine (10-40 mg/kg IP) had little or no effect on performance, while cocaine (3.75-22.5 mg/kg IP) produced dose-related impairment. When each dose of caffeine was combined with 3 mg/kg midazolam, a marked synergism in motor performance impairment occurred. Cocaine plus midazolam produced mainly an additive synergism. The conspicuous synergistic action of caffeine on the motor control deficit produced by midazolam contrasts with the typical antagonism found between the benzodiazepines and methylxanthines when performance is evaluated by psychomotor tests not requiring fine motor control.     

The inhibition of cyclo-oxygenase of rabbit platelets by aspirin is prevented by salicylic acid and by phenanthrolines.

Salicylic acid, 1,10- and 1,7-phenanthroline prevented inhibition by aspirin of platelet aggregation and of generation of thromboxane A2 due to arachidonic acid, to the ionophore A21387, to thrombin and to collagen. Dithiothreitol, another drug which prevents aggregation and formation of thromboxane A2, but only reversibly, failed to interfere with the inhibition by aspirin. Irreversible inhibition by indomethacin and by the substrate analogue 5,8,11,14-tetraynoic acid was also unaffected by salicylic acid or by 1,10-phenanthroline, which thus probably exert a specific interaction with the aspirin-binding site. Inactivation of platelet cyclo-oxygenase with arachidonic acid led to inhibition of the formation of thromboxane A2 and of aggregation due to arachidonic acid itself and to collagen, but barely affected aggregation by thrombin, even though generation of thromboxane A2 was blocked. Use of salicylic acid and of reversible inhibitors of cyclo-oxygenase may help to unravel the mechanism of inhibition due to other agents.     

Local injuries by accidental ingestion of corrosive substances by children

Own data and analysis of previous publications show that situations where accidental ingestion of corrosive substances by children may have happened are frequent, but severe corrosive esophagitis leading to perforation or stricture formation is very rare. In case of suspected esophageal injury, esophagoscopy and glucocorticoid treatment become necessary. The evaluation of the initial symptoms in patients from our own material and from the literature indicates that all children with serious esophageal burns had one or more of the following symptoms: visible burns in the oral cavity, hypersalivation, retching, vomiting, retrosternal or epigastric pain, cardiovascular collaps, airway stenosis. Hence, children with an uncertain history of ingestion and without any of these symptoms need not be treated. After ingestion of liquid substances, but never of dry or granular products, lesions in the esophagus without accompanying burns in the oral cavity were observed. The evaluation of 1158 cases of accidental ingestions of several types of household products and a collection of data from the literature on the causticity of these substances shows that cleaners containing mainly detergents and phosphates (with pH values generally between 9 and 11), and household bleaches on sodium hypochlorite basis are relatively harmless. Drain cleaners (NaOH), decalcifiers (formic acid) and detergents for automatic dish washing machines (metasilicates) are very caustic and are responsible for the majority of serious accidents in children.

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Zusammenfassung Eigenes Zahlenmaterial und eine Durchsicht früherer Veröffentlichungen ergeben, daß Situationen, in denen Kinder versehentlich ätzende Haushaltsmittel zu sich genommen haben (oder haben könnten), häufig sind, daß aber schwere Ösophagusverätzungen mit Perforationen oder Strikturbildung im Kindesalter sehr selten sind. Beim Verdacht auf eine erheblichere Ösophagusverätzung werden Ösophagoskopie und Glukokortikosteroidbehandlung erforderlich. Alle Kinder mit erheblichen Ösophagusverätzungen, über deren Aufnahmestatus in unseren Unterlagen oder in Publikationen Angaben gemacht worden sind, hatten mindestens eines der folgenden Symptome: sichtbare Ätzspuren in Mund und Rachen, Hypersalivation, Würgen, Erbrechen, Schmerzen hinter dem Brustbein oder im Oberbauch, Kreislaufkollaps, Luftwegsstenose. Demnach brauchen Kinder, deren Anamnese nur fraglich ist, und die keines der genannten Symptome haben, nicht behandelt zu werden. Bei trockenen Substanzen waren stets Ätzspuren in der Mundhöhle sichtbar, wenn es zu Ösophagusverätzungen gekommen war; bei Ösophagusschäden durch Flüssigkeiten fehlen gelegentlich Nekrosen in der Mundhöhle. Die Auswertung von 1158 Verätzungsunfällen bei Kindern mit verschiedenen Haushaltsprodukten, und eine Zusammenstellung bereits bekannter, relevanter Daten zeigt, daß Allzweckreiniger auf Detergentien- und Polyphosphat-Basis (in der Regel mit pH-Werten zwischen 9 und 11) und Haushaltsbleichen (Natriumhypochlorit) verhältnismäßig harmlos sind. Reiniger für maschinelles Geschirrspülen (Metasilikate), Abflußreiniger (Natronlauge) und Entkalker (Ameisensäure) sind stark ätzend und verursachen die Mehrzahl der schweren Verätzungsunfälle bei Kindern.

     

冠舒注射液的薄层色谱鉴别及含量测定

报道了冠舒注射液中葛根和元胡的薄层色谱鉴别结果，方法简便。并用分光光度法对其总黄酮的含量进行了测定，以便控制产品质量，结果可靠、重现性好．三批样品含量分别为８．７８３、７．９０６和８．１３４ｍｇ／ｍｌ。