薄层色谱法快筛中药制剂和保健食品12种镇静催眠药

目的建立薄层色谱的方法快速筛查中药制剂或保健食品中非法添加的12种镇静催眠药。方法样品经甲醇提取后,采用硅胶GF254薄层板为固定相,以乙酸乙脂-异丙醇(10:1)为展开剂,展开后置紫外光灯(254nm)处检视。结果在该色谱条件下,氯氮平、三唑仑、艾司唑仑、氯氮卓、奥沙西泮、地西泮、阿普唑仑、马来酸咪达唑仑、劳拉西泮、硝西泮、氯硝西泮出现暗色斑点,扎来普隆显荧光斑点。结论本方法经济、快速简便,可用于快速筛查中药制剂、保健食品中非法添加的镇静催眠类化学药物。     

替代对照品法在镇静安神类药物HPLC快速检验方法中的应用

目的 采用替代对照品法建立镇静安神类药物氯氮卓、马来酸咪达唑仑、硝西泮、艾司唑仑、奥沙西泮、劳拉西泮和阿普唑仑的高效液相色谱快速检验方法。方法 采用Agilent ZORBAX Eclipse Plus C₈色谱柱(4.6 mm×150 mm,5 μm),流动相：0.01 mol·L^-1磷酸二氢钾溶液(pH 2.5)-(甲醇-乙腈1∶1)(57∶43),流速：1.0 mL·min^-1,柱温：30 ℃。采用相对容量因子和紫外光谱相似度双指标进行定性;采用相对校正因子法进行定量分析。结果 在确定的色谱条件下,氯氮?、咪达唑仑、硝西泮、艾司唑仑、奥沙西泮、劳拉西泮和阿普唑仑完全分离;采用紫外光谱相似度和相对容量因子进行定性,结果准确可靠;采用替代对照品法,计算药物的相对校正因子进行含量测定,能有效减少对照品的使用,加快高效液相色谱分析速度。结论 该方法快速、简便、可靠,适用于快速检验镇静安神类药物。     

高效液相色谱法测定人血浆中地西泮、艾司唑仑浓度

目的:建立HPLC法检测人血浆中地西泮、艾司唑仑的浓度.方法:以依利特Hypersil C18高效液相色谱柱为分离色谱柱,地西泮、艾司唑仑互为内标,甲醇-乙腈-水(28:28:54)为流动相,流速1.0mL·min-1,柱温35 ℃,检测波长230nm;结果:地西泮和艾司唑仑分离良好,线性范围分别为0.02μg·mL-...     

UPLC Q－TOF MS法快速检测复方咳喘王胶囊中非法掺入5种化学物质

摘 要 目的：建立超高效液相色谱 飞行时间质谱联用法（UPLC Q－TOF MS）检测复方咳喘王胶囊中非法添加的盐酸二氧丙嗪、马来酸氯苯那敏、磺胺甲噁唑、醋酸泼尼松及甲氧苄啶。方法: 复方咳喘王胶囊用甲醇提取,采用UPLC Q－TOF MS法检测,色谱条件为：Algient ZORBAX SB C₁₈柱(100 mm×2.1 mm,1.8 μm),流动相：10 mmol·L^-1醋酸铵溶液(含0.1%甲酸）－甲醇梯度洗脱,流速：0.3 ml·min^-1 ,柱温：35 ℃,正离子扫描检测。结果: 复方咳喘王胶囊中非法掺入盐酸二氧丙嗪、马来酸氯苯那敏、甲氧苄啶、磺胺甲噁唑及醋酸泼尼松的保留时间和对照品相同,经 Targeted MS/MS法进一步得到快速确证。结论:本方法操作简便,结果可靠,可用于快速确证复方咳喘王胶囊中非法添加的盐酸二氧丙嗪、马来酸氯苯那敏、甲氧苄啶、磺胺甲噁唑及醋酸泼尼松。     

UPLC-MS/MS检测镇静安神类中成药中违禁添加地西泮、氯硝西泮和艾司唑仑

目的建立镇静安神类中成药中添加地西泮、氯硝西泮和艾司唑仑的专属检测方法。方法采用超高效液相色谱-串联四级杆质谱,C₁₈色谱柱（2.1 mm×50 mm,1.7μm）,10 mmol/L乙酸铵溶液-乙腈（90:10）梯度洗脱,流速0.4 ml/min,检测波长254nm;离子源为ESI源,正离子检测,对中成药中添加地西泮、氯硝西泮和艾司唑仑定性、定量检测。结果地西泮、氯硝西泮和艾司唑仑线性范围分别为109.8-878.4、102.1-816.8、106.9～855.2 ng/ml,地西泮、氯硝西泮和艾司唑仑的检出限为分别0.016、2.5×10^-3、2.8×10^-3ng,定量限分别为0.19、8.2×10^-3、9.2×10^-3ng,3种药物平均回收率在95.7%～103.7%之间。结论本方法选择性强、灵敏度高、处理方法简单,测定快速,可用于镇静安神类中成药中添加地西泮、氯硝西泮和艾司唑仑的测定。     

HPLC法测定人血浆中氯氮平浓度

目的 建立测定人血浆中氯氮平高效液相色谱法。方法 血浆样品经适当处理,色谱柱为Vova-pak C₁₈柱,流动相为0.5%三乙胺溶液-乙腈(74∶26,v/v),流速1 ml·min^-1,检测波长215 nm,安定为内标。结果 测定方法在50～1600μg·ml^-1范围内,氯氮平线性关系良好(r=0.9992);日内、日间相对标准误差(RSD)在3.6%～5.7%之间。结论 本方法快速、简便、准确,可用于血药浓度监测。     

HPLC法测定人血浆中阿塞那平的含量

摘 要 目的:建立测定人血浆中阿塞那平含量的HPLC法。方法: 色谱柱：DiamonsilC₁₈(250 mm×.6 mm,5 μm)反相柱;柱温：25℃;流动相：乙腈-甲醇-缓冲液（15∶55∶30）;流速：1.0 ml·min^-1;检测波长：254 nm;内标：氯氮平。结果:阿塞那平血浆浓度在50～5 000 μg·L^-1范围内线性关系良好(r=0.999 1),平均提取回收率为87.32%,日内RSD小于4.86%;日间RSD小于8.00%。结论:该方法快速、简便,结果准确,可以用于阿塞那平的临床研究。     

高效液相色谱法同时测定镇静安神类中成药及保健食品中非法添加5种西药成分

目的建立高效液相色谱法-二极管阵列检测器同时分析测定镇静安神类中成药及保健食品中非法添加5种西药成分（苯巴比妥、艾司唑仑、阿普唑仑、三唑仑、地西泮）。方法采用Agela Venusil MP-C18（4.6 mm×150 mm,5μm）色谱柱;流动相为乙腈-体积分数0.5%甲酸（33∶67）;流速：1.0 ml.min^-1;检测波长为254 nm,同时进行DAD全波长扫描（190-400 nm）;柱温：30℃。结果 5种对照化学药在较宽的浓度范围内,峰面积和浓度有良好的线性关系（r≥0.9999）。检出限为1.0-33.2μg,定量限为3.4-110.7μg。结论本方法简便快速准确,重复性好,适用于基层药检机构,可作为镇静安神类中成药及保健食品中非法添加上述5种西药成分的快速筛查方法。     

LC/MSn法同时检测人尿液中艾司唑仑、阿普唑仑和三唑仑

目的研究三氮唑苯并二氮类药物的质谱断裂规律,建立可同时检测人尿液中艾司唑仑、阿普唑仑和三唑仑的液相色谱-质谱(LC/MSⁿ)联用法。方法用LC/MSⁿ技术,同时对3种三氮唑苯二氮类药物进行色谱分离及质谱鉴定,并用质谱解析软件探讨该类化合物的裂解规律。结果3种药物的［M+H］⁺准分子离子均可生成脱去1分子N₂和1个Cl原子的特征碎片离子,其最低检测限小于0.5 ng·mL^-1。结论该方法快速、灵敏、准确,完全适用于法医学和临床用药过量案例或病例的定性分析。     

宁心宝胶囊指纹图谱研究及4种核苷类成分的含量测定

摘 要 目的： 研究宁心宝胶囊的HPLC指纹图谱,并建立同时测定宁心宝胶囊中尿嘧啶、尿苷、腺嘌呤、腺苷含量的方法。方法: 采用Agilent Zorbax SB Aq C₁₈色谱柱（250 mm×4.6 mm,5 μm）,甲醇 0.05 mol·L^-1磷酸二氢钾水溶液为流动相,梯度洗脱,流速为1.0 ml·min^-1,检测波长为212 nm（指纹图谱）、260 nm（含量测定）,柱温为30 ℃。对10 批宁心宝胶囊进行了指纹图谱及含量测定研究,采用中药色谱指纹图谱相似度评价软件进行分析。结果: 建立了宁心宝胶囊的HPLC 指纹图谱,标定了10个共有色谱峰。4种核苷类成分的分离度良好。结论:此方法简便、可靠,指纹图谱结合含量测定可以更好地控制宁心宝胶囊的内在质量。     

Efficacy of gut lavage,hemodialysis, and hemoperfusion in the therapy of paraquat or diquat intoxication

Clinical and in vitro investigations were carried out to test the efficacy of gut lavage, hemodialysis, and hemoperfusion in the treatment of poisoning with paraquat or diquat. In a patient suffering from diquat intoxication 130 times more diquat was removed by gut lavage 30 h after ingestion than was removed by complete aspiration of the gastric contents.Determination of in vitro clearances for paraquat and diquat by hemodialysis showed that, at serum concentrations of 1–2 ppm, such as are frequently encountered in poisoning in man, toxicologically relevant quantities of herbicide cannot be removed from the body. At a concentration of 20 ppm, on the other hand, hemodialysis proved to be effective, the clearance being 70 ml/min at a blood flow rate of 100 ml/min. The efficacy of hemoperfusion with coated activated charcoal was on the whole better. Especially at concentrations around 1–2 ppm, the clearance values for hemoperfusion were some 5–7 times higher than those for hemodialysis.In a patient suffering from paraquat poisoning, both hemodialysis as well as hemoperfusion were carried out. The in vitro results could be confirmed: At serum concentrations of paraquat less than 1 ppm no clearance could be obtained by hemodialysis while by hemoperfusion with activated charcoal quite high clearance values were measured and the serum level dropped down to zero.

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Zusammenfassung Klinische Untersuchungen und Laboratoriumsversuche wurden durchgeführt, um die Wirksamkeit von Darmspülung, Hämodialyse und Hämoperfusion bei Paraquat- und Deiquat-Vergiftungen zu prüfen.Bei einem Patienten wurde 30 Std nach Deiquat-Aufnahme durch Darmspülung 130mal mehr Deiquat entfernt als durch vollständige Aspiration des Mageninhaltes. In vitro-Versuche ergaben, daß bei Blutserumkonzentrationen von 1–2 ppm, die bei Vergiftungen oft gemessen werden, durch Hämodialyse keine toxikologisch relevanten Paraquat- oder Deiquat-Mengen entfernt werden können. Dagegen erwies sich die Hämodialyse bei 20 ppm und einer Blutumlaufgeschwindigkeit von 100 ml/min mit einer Clearance von 70 ml/min als wirksam. Die Hämoperfusion mit beschicheter Aktivkohle war in diesen Versuchen aber eindeutig überlegen, denn insbesondere bei Konzentrationen um 1–2 ppm waren die Clearance-Werte 5–7mal höher als bei der Hämodialyse.Die in vitro-Ergebnisse wurden bei einem Patienten mit einer Paraquat-Vergiftung bestätigt: Bei Konzentrationen unter 1 ppm war die Hämodialyse wirkungslos, während durch Hämoperfusion relativ hohe Clearance-Werte erreicht wurden, so daß der Serumspiegel rasch unter die Nachweisgrenze abfiel.

     

In vitro studies on sterically stabilized liposomes (SL) as enzyme carriers in organophosphorus (OP) antagonism

This study describes a new approach for organophosphorous (OP) antidotal treatment by encapsulating an OP hydrolyzing enzyme, OPA anhydrolase (OPAA), within sterically stabilized liposomes. The recombinant OPAA enzyme was derived from Alteromonas strain JD6. It has broad substrate specificity to a wide range of OP compounds: DFP and the nerve agents, soman and sarin. Liposomes encapsulating OPAA (SL)* were made by mechanical dispersion method. Hydrolysis of DFP by (SL)* was measured by following an increase of fluoride ion concentration using a fluoride ion selective electrode. OPAA entrapped in the carrier liposomes rapidly hydrolyze DFP, with the rate of DFP hydrolysis directly proportional to the amount of (SL)* added to the solution. Liposomal carriers containing no enzyme did not hydrolyze DFP. The reaction was linear and the rate of hydrolysis was first order in the substrate. This enzyme carrier system serves as a biodegradable protective environment for the recombinant OP-metabolizing enzyme, OPAA, resulting in prolongation of enzymatic concentration in the body. These studies suggest that the protection of OP intoxication can be strikingly enhanced by adding OPAA encapsulated within (SL)* to pralidoxime and atropine.     

Steroidal sapogenin contents in some domestic plants

In order to find out the values of the steroid resources for the future use. the compositions and contents of steroidal sapogenins from 13 domestic plants have been investigated. As a result,Dioscorea nipponica, D. quinqueloba andSmilax china were found to have large amount of diosgenin. And pennogenin inTrillium kamtschaticum andParis verticillata, yuccagenin inAllium fistulosum, hecogenin inAgave americana and neochlorogenin inSolanum nigum were appeared to be major steroidal sapogenins.     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

Aquatic Insects and Trace Metals: Bioavailability,Bioaccumulation, and Toxicity

Abstract

The uptake of metals from food and water sources by insects is thought to be additive. For a given metal, the proportions taken up from water and food will depend both on the bioavailable concentration of the metal associated with each source and the mechanism and rate by which the metal enters the insect. Attempts to correlate insect trace metal concentrations with the trophic level of insects should be made with a knowledge of the feeding relationships of the individual taxa concerned. Pathways for the uptake of essential metals, such as copper and zinc, exist at the cellular level, and other nonessential metals, such as cadmium, also appear to enter via these routes. Within cells, trace metals can be bound to proteins or stored in granules. The internal distribution of metals among body tissues is very heterogeneous, and distribution patterns tend to be both metal and taxon specific. Trace metals associated with insects can be both bound on the surface of their chitinous exoskeleton and incorporated into body tissues. The quantities of trace meals accumulated by an individual reflect the net balance between the rate of metal influx from both dissolved and particulate sources and the rate of metal efflux from the organism. The toxicity of metals has been demonstrated at all levels of biological organization: cell, tissue, individual, population, and community. Much of the literature pertaining to the toxic effects of metals on aquatic insects is based on laboratory observations and, as such, it is difficult to extrapolate the data to insects in nature. The few experimental studies in nature suggest that trace metal contaminants can affect both the distribution and the abundance of aquatic insects. Insects have a largely unexploited potential as biomonitors of metal contamination in nature. A better understanding of the physico-chemical and biological mechanisms mediating trace metal bioavailability and exchange will facilitate the development of general predictive models relating trace metal concentrations in insects to those in their environment. Such models will facilitate the use of insects as contaminant biomonitors.