柱前衍生化RP-HPLC法测定肌醇片剂的含量

目的：采用柱前衍生化RP－HPLC法测定肌醇片的含量。方法：以苯甲酰氯为衍生化试剂，ODS反相柱为固定相，甲醇－水（85：15）为流动相，检测波长230nm.结果：衍生化反应迅速，制剂辅料和可能降解产物不干扰测，制剂的平均回收率为100．2％，RSD为1．8％，结论：该方法测定结果准确，专属性强，适用于肌醇片剂的质量控制。     

醋酸环丙孕酮／炔雌醇复方片剂在人体的药代动力学

目的建立人血浆中醋酸环丙孕酮的HPLC—ESI—MS测定方法和丹酰氯衍生化血浆中炔雌醇的HPLC—APCI—MS测定方法,测定女性志愿者口服复方醋酸环丙孕酮片1片后的药代动力学参数,并对受试制剂和参比制剂的生物等效性进行评价。方法血浆样品中的炔雌醇以乙酸乙酯提取后,与丹酰氯发生衍生化反应,进行HPLC—APCI—MS分析,流动相为10mmol·L-1乙酸铵缓冲液（1％甲酸）-甲醇（3：97）。检测离子分别为m／z530．3（炔雌醇的丹酰氯衍生物）、m／z404．3（内标,对羟基联苯的丹酰氯衍生物1。结果在10．43～625．8Pg·ml-1范同内炔雌醇的丹酰氯衍生物与内标的丹酰氯衍生物峰面积比值与浓度呈良好的线性关系,最低定量限为10．43pg·ml-1结论本实验建立的分析方法灵敏、准确、简便,且统计学结果表明两种制剂生物等效。     

盐酸美金刚胶囊的丹磺酰氯柱前衍生化-HPLC法测定

建立了柱前衍生化-HPLC法测定盐酸美金刚胶囊的含量.样品与丹磺酰氯在25℃、避光衍生化反应90 min后测定.采用C_8 色谱柱,以磷酸盐缓冲液(pH 3.0)-乙腈(25:75)为流动相,检测波长218 nm.在5～180 μg/ml浓度范围内线性关系良好(r=0.999 9),日内和日间RSD为1.15%和0.48%,平均回收率为99.7%～101.1%,衍生化产物在17h内稳定.     

HPLC—UV／ESI—MS法分析丹参不同提取组分

目的对丹参4种不同组分进行HPLC-UV-MS分析，获得各组分的HPLC特征图谱并对各特征峰进行初步MS鉴定，同时定量测定指标成分丹参素、丹酚酸B、丹参酮ⅡA和隐丹参酮的含量，以便更深入的探讨其在抗动脉粥样硬化作用的物质基础及谱效关系。方法采用Hedera ODS-2色谱柱（4．6min×250mm，5μm），0．5％甲酸水溶液-乙腈（0min，80：20；50min，15：85）梯度洗脱，流速：1．0mL·min^-1，检测波长：280nm，建立以上各组分的HPCL指纹图谱，同时对各特征峰进行离子范围为150-750正负源ESI-MS总离子扫描，对相应特征峰的特征离子进行鉴定，用分子离子检测模式（SIR）分别对丹参素、丹酚酸B、丹参酮ⅡA和隐丹参酮进行定量测定。结果所得HPLC特征图的特征峰峰形尖锐、对称，均达到基线分离；14个特征峰经质谱鉴定，对照有关文献可初步确定其成分；丹参素、丹酚酸B、丹参酮ⅡA和隐丹参酮分别在0．05-10．0、0．05-20．0、0．05-20、0．05-20μg·mL^-1与峰面积呈良好的线性关系（r≥0．9998），平均加样回收率分别为98．1％、99．0％、98．9％、99．5％。结论所得4种组分的HPLC特征图谱适合下一步的译效学及相关药理活性成分筛选研究；定量测定方法准确可靠，适合丹参药材中上述成分的含量测定；所建立的HPLC特征图谱能为丹参药材指纹图谱的建立提供依据。     

乳块消胶囊质量控制方法探讨

采用HPLC法测定乳块消胶囊中原儿茶醛含量：C18柱，甲醇-0．05mol／L磷酸盐缓冲液（pH=3）=20：80为流动相，检测波长230nm，原儿茶醛保留时间8min；采用TLC法鉴别胶囊中王不留行和川楝子。     

高效液相色谱法测定呋布西林钠的含量及有关物质

目的探讨用高效液相色谱（HPLC）法测定呋布西林钠的含量及有关物质。方法采用C18柱，以磷酸盐缓冲液（0.1mol／L磷酸二氢钾溶液，用磷酸调节pH值至3.5）-乙腈（80：20）为流动相A，以磷酸盐缓冲液（0．1mol／L磷酸二氢钾溶液，用磷酸调节pH值至3．5）-己腈（75：25）为流动相B，对含量测定以流动相B等度洗脱，对有关物质测定以线性梯度洗脱，流速为1．0mL／min，检测波长为225nm。结果呋布西林钠质量浓度的线性范围为0．02256～0．9024mg／mL，r=0．9999，平均加样回收率为99.8％，RSD为0．60％（n=6）。结论HPLC法简便、准确、灵敏度高，可同时对产品的含量及有关物质进行准确监控。     

阿莫西林/克拉维酸钾原料及制剂中有关物质测定方法的比较

目的建立两种HPLC线性梯度洗脱测定阿莫西林／克拉维酸钾有关物质的方法，并对其进行比较。方法两种方法均采用C18柱，流速1．0mi／min，所用流动相为磷酸盐缓冲液：乙腈色谱系统。方法一中流动相A为0．05mol／L磷酸盐缓冲液（pH5．0）；乙腈（99：1），流动相B为0．05mol／L磷酸盐缓冲液（pH5．0）：乙腈（80：20）；方法二中流动相A为0．01mol／L磷酸盐缓冲液（pH6．0），流动相B为0．01mol／L磷酸盐缓冲液（pH6．0）：乙腈（20：80）。两种方法的梯度变化不同。方法一和方法二的检测波长分别为254和215nm。结果两种方法的线性范围、检测限及测定结果基本一致。结论两种方法准确，专属性强，灵敏度高，适用于阿莫西林／克拉维酸钾中有关物质测定，且方法一的稳定性优于方法二。     

复方α-酮酸片中氨基酸的柱前衍生化-HPLC法测定

采用柱前衍生化法同时测定复方α酮酸片中——L-醋赖氨酸、L-苏氨酸、L-色氨酸、L-组氨酸、L-酪氨酸五种氨基酸的含量。采用ODS柱，以流动相乙腈-水（1：1）和0．14mol／L磷酸盐缓冲液（pH8．2）梯度洗脱，检测波长360nm。衍生化试剂为2，4-二硝基氯苯。五种氨基酸的平均回收率为99．6％～100．9％，RSD小于1．1％。     

旋光法测定硫酸丁胺卡那霉素注射液含量

复方新诺明中磺胺甲基异唑溶出度以pH6．8磷酸盐缓冲液为介质，用双波长紫外分光光度法测定，标准曲线相关性为0．9994，平均回收率为101．76％，CV％为1．80％，SMZ溶出速率A药（江浦药厂）为0．0275／min、B药（光华药业公司）为0．0487／min，Td：A药为27．8min、B药为16．5min，T80：A药为50．8min、B药为28.2min。     

高效液相色谱法测定牛磺酸颗粒的含量

目的：建立高效液相色谱（HPLC）法测定牛磺酸颗粒的含量。方法：采用2，4-二硝基氟苯作为柱前衍生化试剂，以C，。色谱柱为分析柱，乙腈-水-磷酸盐缓冲液（pH7．0）（20：10：70）为流动相，检测波长为360nm，以峰面积外标法计算。结果：牛磺酸在1．0～3．0μg范围内线性关系良好（r=0．9999），测得平均回收率为99．80％，RSD为0．21％，衍生物在24h内的稳定性良好，最低检出量为0．02ng。结论：本方法简单，快速，专属性强，灵敏度高，重现性好，结果准确，可靠。     

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.     

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.     

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.     

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.