气相色谱法测定细辛脑中的有机溶剂残留量

目的 建立气相色谱法测定细辛脑中四氢呋喃、乙醇、甲苯的残留量。方法 采用SUPELCOWAX-10的毛细管石英色谱柱（30mm×0．53mm，1．0μm）；载气：氮气；以N，N-二甲基甲酰胺为溶剂；柱温：60℃，保持5min，以30℃·min^-1。升温至180℃，维持1min；进样口温度：250℃；检测器温度：250℃（FID）。结果 四氢呋喃在0．634～211．2μg·mL^-1内线性关系良好，r＝0．999 1 （n＝6），最低检测限为0．190μg·mL^-1，回收率为98．8％（RSD=4．3％）；乙醇在1．032～206．4μg·mL^-1内线性关系良好，r＝0．9992（n＝6），最低检测限为0．310μg·mL^-1,回收率为97．7％（RSD=3．O％）；甲苯在0．604～36．24μg·mL^-1内线性关系良好，r＝0．9995（n＝6）），最低检测限为0．174μg·mL^-1，回收率为100．3％（RSD＝0．7％）：结论本方法可用于细辛脑中四氢呋喃、乙醇和甲苯的残留量测定。     

HPLC-ELSD测定复方黄芪心通颗粒中黄芪甲苷的含量

目的：建立复方黄芪心通颗粒中黄芪甲苷的HPLC—ELSD含量测定的方法。方法：色谱柱：AgelentSB—C18（250mm×4．6mm,5μm）,柱温：35℃,流动相：乙腈-水-四氢呋喃（27：70：3）,检测器：蒸发光散射检测器（漂移管温度40℃）。结果：黄芪甲苷在1．32～6．60μg范围内呈良好的线性关系,r=0．9994,平均回收率为97．2％,RSD％为1．08％。结论：方法简便,结果准确,重复性好,可用于该制剂的质量控制。     

HPLC法测定宽胸舒气化滞丸中咖啡酸的含量

目的：建立宽胸舒气化滞丸中咖啡酸的含量测定方法。方法：采用HPLC法测定，色谱柱为十八烷基硅烷键合硅胶填充柱（4．6mm×250mm，5μm），柱温40℃，流动相为乙腈-0．04％磷酸溶液（11：89），流速为1．0mL·min^-1，检测波长为325nm。结果：咖啡酸在0．0516μg-1．032μg（r=0．9999）范围内呈良好的线性关系，平均回收率为100．57％，RSD为1．75％（n=6）。结论：实验表明，该方法准确，灵敏度高，重现性好。     

GC测定马来酸伊索拉定原料中二氧六环和2-甲氧基乙醇残留量

目的建立GC测定马来酸伊索拉定原料中二氧六环和2-甲氧基乙醇的残留量。方法样品以二甲基甲酰胺溶解,色谱柱为HP-INNOWAX毛细管柱（30m×0．53mm,1μm）,检测器为氢火焰离子化检测器,柱温为程序升温,初始柱温为40℃,进样口温度为200℃,检测器温度为250℃。结果二氧六环和2-甲氧基乙醇分别在7．6～76μg·mL^-1和1．0～10gg·mL^-1内线性关系良好p分别为0．9999和0．9984）,平均回收率分别为94．7％（RSD=3．7％）和98．2％（RSD=3．9％）,检测限分别为0．9μg·mL^-1和0.3μg·mL^-1。结论本方法灵敏度高、准确度好,可用于马来酸伊索拉定原料中二氧六环和2-甲氧基乙醇的残留量测定。     

基于二进制信息粒的数据挖掘算法研究

目的：建立盐酸氨溴索原料药中醋酸残留量的测定方法。方法：采用离子色谱法，离子色谱条件：采用Ionpac AG14A，AS14A阴离子色谱柱；淋洗液：8mmol·L^-1Na2CO3／1mmol·L^-1NaHCO3；ASRS-ULTRA 4mm自动抑制循环模式，抑制电流50mA；电导检测池温度：35℃；进样量：25μL。结果：醋酸在1～40mg·L^-1浓度内呈良好的线性关系（r=0．9993）；回收率为99．47％～101．22％（RSD≤〈1．2％，n=3）；醋酸的检测限为0．05mg·L-1。结论：本方法简单、快捷，可以肝于盐酸氨溴索中醋酸残留量的控制。     

聚乙二醇化重组人干扰素β-1a注射液中游离聚乙二醇残留量的测定

目的对聚乙二醇化重组人干扰素β-1a（PEG-rhIFN-β-1a）注射液中的残留聚乙二醇丁醛（PEG）进行方法学研究。方法采用Phenomenex JupiterC4色谱柱,流动相：A相,0．1％三氟乙酸．水溶液;B相,0．1％三氟乙酸一乙腈溶液,梯度洗脱;流速：1.0mL·min^-1,柱温为25℃,蒸发光检测器,漂移管温度为113．0℃,栽气流速为3．1L．min。结果PEG在0.6～2.0μg·mL^-1内线性良好,相关系数为0．9984,检出限为0.20μg,定量限为0．40gg,精密度、稳定性和重复性试验的RSD均＜2．O％,平均回收率为96％～100％。结论运用该方法对PEG-rhIFN-β-1a注射液中游离PEG残留量测定,残留量＜1.0％。     

5—O-甲基-myo-肌醇的含量测定方法

目的建立5-O-甲基-myo-肌醇含量测定的方法;方法色谱柱（Agilent zorbax NH2,4．6×250mm,5μm）、流动相（乙腈：水=75：25）、流速（1．0mL·min^-1）、柱温（30℃）、ELSD（gain=6,Barm3．5,漂移管温度=40℃）;结果5-O-甲基-myo-肌醇进样量在2．0μg～40μg的范围里线性（r=0．9996）良好,平均回收率为99．51％,RSD值为2．28％（n=9）;结论本方法操作简便,重现性好,结果准确。     

顶空气相色谱法测定盐酸普鲁卡因中的残留溶剂

目的：建立盐酸普鲁卡因中乙醇、丙酮残留量的测定方法。方法：采用顶空气相色谱法,以水为溶解介质,色谱柱为DB一1301石英毛细管柱,柱温80℃,检测器为FID,检测器温度为250℃,进样口温度为150℃,结果：乙醇、丙酮的线性范围分别为0．025～2．0nag·ml-1（r=0．9999）和0．025—2．0mg·ml-1（r=0．9999）;平均回收率分别为99．6％（RSD=0．6％）和99．5％（RSO：1．1％）;定量限分别为4．79μg·ml-1和3．01μg·ml-1。结论：方法简单、准确,可用于盐酸普鲁卡因中乙醇和丙酮残留量的测定。     

SPE-UPLC-ELSD法测定柴胡中柴胡皂苷a、d的含量

目的：应用超高效液相色谱-蒸发光散射（UPLC—ELSD）检测柴胡中柴胡皂苷a、d的含量。方法：采用Waters Acquity UPLC BEH C18色谱柱（2．1mm×100mm,1．7μm）;以乙腈（A）-水（B）为流动相梯度洗脱（0－3min,43％A;3～9min,43％A→63％A）;流速：0．2mL．min-1：柱温：30℃;ELSD检测器漂移管温度为40℃,气体压力为40psi,测定柴胡中柴胡皂苷a、d的含量。结果：柴胡中柴胡皂苷a在浓度为64．2-385．2Dg·mL—1（r=0．9994）内线性范围良好：柴胡皂苷d在浓度为67．3～403．8μg·mL-1（r=0．9992）内线性范围良好。结论：该方法简便、灵敏、可靠、准确、重现洼好,可作为柴胡的质量控制方法。     

HPLC-RID法测定吸附无细胞百白破联合疫苗中甘油的残留量

目的:建立高效液相色谱-示差折光(HPLC-RID)法测定吸附无细胞百白破联合疫苗中甘油残留量的方法,为其检测提供参考.方法:采用NH2色谱柱(250 mm×4.6 mm,5μm),以乙腈-水(85:15)为流动相,柱温30℃,RID检测器温度35℃,流速1.0 mL·min-1.结果:甘油在43.5～2173.0μg...     

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.