一测多评法同时测定北青龙衣药材中胡桃醌和胡桃酮的含量

目的:建立同时测定北青龙衣药材中胡桃醌、胡桃酮含量的方法。方法:采用高效液相色谱法,以胡桃醌为内参物,计算其对胡桃酮的相对校正因子(RCF),通过RCF计算北青龙衣药材中胡桃酮的含量;以外标法测定的胡桃酮含量作实测值,采用夹角余弦法比较一测多评法的计算值与实测值的差异。结果:胡桃醌、胡桃酮检测质量浓度线性范围分别为7.6~76.0μg/mL(r=0.999 0)、8.2~82.0μg/mL(r=0.999 4);精密度、稳定性、重复性试验的RSD<3.0%;加样回收率分别为95.37%~97.94%(RSD=1.04%,n=6)、99.13%~100.10%(RSD=0.33%,n=6)。计算值与实测值之间的夹角余弦值为0.999 84,两者差异无统计学意义(P>0.05)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于北青龙衣药材中胡桃醌、胡桃酮含量的同时测定。     

HPLC法测定不同产地地龙中尿嘧啶、次黄嘌呤、尿苷、肌苷的含量

目的:测定不同产地、品种的地龙药材中尿嘧啶、次黄嘌呤、尿苷、肌苷的含量,建立地龙质量控制的客观指标。方法:用0.9%生理盐水超声提取地龙药材,采用反相高效液相色谱法,Waters Symmetry C₁₈色谱柱（150mm×4.6mm,5μm）,以0.01mol·L^-1磷酸二氢钾溶液和50%甲醇为流动相,流速为0.8ml·min^-1,梯度洗脱,检测波长254nm,柱温27℃,同时测定尿嘧啶、次黄嘌呤、尿苷、肌苷等4种成分的含量。结果:尿嘧啶的线性范围为0.75～24.00μg·ml^-1（r=0.9993）,平均回收率99.82%,RSD=2.34%（n=6）;次黄嘌呤的线性范围2.50～80.00μg·ml^-1（r=0.9992）,平均回收率101.93%,RSD=1.45%（n=6）;尿苷的线性范围1.25～40.00μg·ml^-1（r=0.9992）,平均回收率97.53%,RSD=1.73%（n=6）;肌苷的线性范围5.00～160.00μg·ml^-1（r=0.9991）,平均回收率102.06%,RSD=2.44%（n=6）。结论:该方法重复性,回收率好,可用于地龙药材中尿嘧啶等4种成分的含量测定。     

一测多评法同时测定降脂减肥保健品中儿茶素类活性成分的含量

目的:建立同时测定减肥降脂保健品中儿茶素类活性成分含量的方法。方法:采用高效液相色谱法,以表没食子基儿茶素没食子酸酯(EGCG)为内标,计算其与没食子儿茶素(EGC)、儿茶素(C)、表儿茶素(EC)、没食子基儿茶素没食子酸酯(GCG)和没食子酰表儿茶素(ECG)的相对校正因子(RCF),通过RCF计算样品中EGC、C、EC、GCG、ECG的含量,以外标法测定的EGC、C、EC、GCG和ECG含量作实测值;采用向量夹角余弦法评估实测值与计算值之间的相似性。结果:EGC、C、EC、EGCG、GCG、ECG检测质量浓度线性范围分别为0.006 5~0.130 5 mg/m L(r=0.999 8)、0.000 5~0.010 7 mg/m L(r=0.999 7)、0.002 0~0.040 0mg/m L(r=0.999 9)、0.015 3~0.305 3 mg/m L(r=0.999 8)、0.000 8~0.015 5 mg/m L(r=0.999 8)、0.004 0~0.079 2 mg/m L(r=0.999 9);精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为95.07%~100.35%(RSD=1.94%,n=6)、95.24%~101.87%(RSD=2.79%,n=6)、96.08%~103.86%(RSD=3.01%,n=6)、97.51%~101.06%(RSD=1.45%,n=6)、96.01%~101.66%(RSD=2.27%,n=6)、96.20%~102.89%(RSD=2.71%,n=6)。实测值与计算值差异无统计学意义(P>0.05)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于减肥降脂保健品中儿茶素类活性成分的含量测定。     

一测多评法同时测定山银花药材中5种皂苷类成分的含量

目的:建立同时测定山银花药材中5种皂苷类成分含量的方法。方法:采用高效液相色谱法,以灰毡毛忍冬皂苷乙为内标,计算其对灰毡毛忍冬皂苷甲、川续断皂苷乙、灰毡毛忍冬次皂苷甲和灰毡毛忍冬次皂苷乙的相对校正因子(RCF),通过RCF计算上述4种皂苷类成分的含量;以外标法测定的上述皂苷类成分含量作实测值,比较计算值与实测值的差异。结果:灰毡毛忍冬皂苷甲、灰毡毛忍冬皂苷乙、川续断皂苷乙、灰毡毛忍冬次皂苷甲和灰毡毛忍冬次皂苷乙检测进样量线性范围分别为0.316~6.32μg(r=0.997 3)、0.453~9.06μg(r=0.998 2)、0.231~4.62μg(r=0.999 6)、0.342~6.84μg(r=0.998 4)、0.147~2.94μg(r=0.996 1);精密度、稳定性、重复性试验的RSD<2.0%;加样回收率试验的RSD分别为97.74%~104.51%(RSD=2.37%,n=6)、96.70%~103.20%(RSD=2.37%,n=6)、96.12%~103.61%(RSD=2.45%,n=6)、98.80%~104.70%(RSD=2.32%,n=6)、99.21%~102.92%(RSD=1.39%,n=6)。计算值与实测值差异无统计学意义(P>0.05)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于山银花药材中5种皂苷类成分含量的同时测定。     

小儿清热止咳颗粒剂质量标准研究

目的：制订小儿清热止咳颗粒剂质量标准。方法：对杏仁药材进行了薄层色谱鉴别,紫外分光光度法测定了总黄酮的含量,结果：回收率为98．45％（RSD％＝1．83％,n=6),线性范围为2．72ug/ml-19.04ug/ml,线性关系r=0.9998,重复线RSD＝1．09％（n=6),精密度RSD＝0．91％（n=6),结论：方法稳定,可靠,可作为该制剂的质量控制方法之一。     

RP-HPLC同时测定治胃丸中2种有效成分含量

目的建立反相高效液相色谱(RP-HPLC)同时测定治胃丸中橙皮苷、芍药苷含量的方法,并分析其可行性。方法选用Synergi Hydro-RP C_(18)色谱柱(250 mm×4.6 mm,4μm),以乙腈和0.1%碳酸溶液为流动相进行梯度洗脱,流速1.0 ml/min,检测波长230 nm,柱温35℃。结果橙皮苷和芍药苷质量浓度线性范围分别为8.35～83.52μg/ml(r=0.999 1)、1.51～15.1μg/ml(r=0.999 8);该测定方法精密度、稳定性、重复性均符合要求;橙皮苷、芍药苷平均加样回收率分别为99.5%(RSD=2.4%,n=6)、98.3%(RSD=1.9%,n=6),具有较高的准确度;各批号治胃丸中橙皮苷含量5.38～5.82 mg/g,芍药苷含量1.49～1.70 mg/g。结论 RP-HPLC操作简便,专属性强,精密度高,且具有较好的稳定性和重复性,可同时测定治胃丸中橙皮苷、芍药苷的含量,可用于治胃丸的质量控制。     

HPCE法测定金银花药材中木犀草苷、槲皮素和金丝桃苷的含量

目的:建立同时测定金银花药材中木犀草苷、槲皮素和金丝桃苷含量的方法。方法:采用高效毛细管电泳法。毛细管柱为石英毛细管柱,检测波长为360 nm,分离电压为20 k V,进样方式为电动进样,进样电压为15 k V,进样时间为5 s,操作温度为25℃,缓冲溶液为60 mmol/L四硼酸钠-50 mmol/L碳酸钠-50 mmol/L丙羟基-β-环糊精(p H 9.2)。结果:木犀草苷、槲皮素和金丝桃苷检测质量浓度线性范围分别为0.06~0.56 mg/m L(r=0.988 1)、0.08~0.56 mg/m L(r=0.989 2)、0.06~0.49 mg/m L(r=0.979 6);精密度、稳定性、重复性的RSD<2.0%;加样回收率分别为96.12%~99.77%(RSD=1.29%,n=6)、95.90%~98.35%(RSD=0.89%,n=6)、94.07%~97.45%(RSD=1.33%,n=6)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于金银花药材中木犀草苷、槲皮素和金丝桃苷含量的同时测定。     

化风丹药母指纹图谱的建立及不同发酵时间样品中7种核苷类成分的含量测定

目的:建立化风丹药母的指纹图谱,并测定不同发酵时间样品中7种核苷类成分的含量。方法:采用高效液相色谱法(HPLC),色谱柱为Pntulips BP-C18,流动相为甲醇-水(梯度洗脱),流速为0.8 mL/min,检测波长为260 nm,柱温为35℃,进样量为10μL。以黄嘌呤为参照,绘制12批化风丹药母的HPLC指纹图谱;采用《中药色谱指纹图谱相似度评价系统(2012版)》进行相似度评价,确定共有峰;同法测定不同发酵时间(0、1、2、3、4周)样品中尿嘧啶、次黄嘌呤、黄嘌呤、尿苷、肌苷、鸟苷、胸苷的含量。结果:12批化风丹药母共有8个共有峰,相似度为0.712~0.954;指认了7种成分,分别为尿嘧啶、次黄嘌呤、黄嘌呤、尿苷、肌苷、鸟苷、胸苷。不同发酵时间样品中上述7种成分检测质量浓度的线性范围分别为0.87~8.7μg/mL(r=0.9996)、1.51~15.1μg/m L(r=0.9997)、6.08~60.8μg/m L(r=0.9995)、1.52~15.2μg/m L(r=0.9996)、1.82~18.2μg/mL(r=0.9996)、1.48~14.8μg/m L(r=0.9996)、1.63~16.3μg/mL(r=0.9993);定量限分别为0.0274、0.0763、0.2504、0.1723、0.1011、0.0783、0.0842μg/mL,检测限分别为0.0087、0.0255、0.0079、0.0841、0.0357、0.0269、0.0275μg/m L;精密度、重复性、稳定性(12 h)试验的RSD均小于3%;加样回收率分别为94.16%~100.16%(RSD=2.24%,n=6),93.87%~100.65%(RSD=2.67%,n=6),93.52%~99.66%(RSD=2.30%,n=6),93.67%~98.24%(RSD=1.89%,n=6),96.00%~102.18%(RSD=1.96%,n=6),94.62%~101.54%(RSD=2.82%,n=6),97.72%~104.56%(RSD=2.97%,n=6)。发酵0~4周时,上述7种成分及总核苷的含量分别为0.042~0.232、0.027~0.181、0.039~0.651、0.026~0.225、0.034~0.111、0.009~0.124、0.079~0.099、0.647~1.292 mg/g;发酵1~4周时的尿嘧啶、次黄嘌呤、黄嘌呤及总核苷的含量均较发酵0周时显著升高,而尿苷、肌苷、鸟苷的含量较发酵0周时显著降低。结论:所建指纹图谱特征性强且操作简便,可用于化风丹药母的质量控制;含量测定方法准确、可靠,可用于同时测定其中7种核苷类有效成分的含量;化风丹药母中的核苷类成分含量受发酵时间的影响。     

UPLC法同时测定盐酸阿糖胞苷原料药的含量和有关物质

目的:建立同时测定盐酸阿糖胞苷原料药的含量和有关物质的方法。方法:采用超高效液相色谱法。色谱柱为Inertsil ODS-3 C18,流动相为磷酸盐缓冲液-甲醇(梯度洗脱),流速为0.8 ml/min,检测波长为254 nm,柱温为40Ⅴ,进样量为10μl。结果:尿嘧啶、尿苷、阿糖尿苷、盐酸阿糖胞苷检测质量浓度分别在0.100 8²0.16、0.120.16、0.1²0.12、0.095 620.12、0.095 6¹9.12、0.119.12、0.1²0.004μg/ml范围内与各自峰面积积分值呈良好的线性关系(r=0.999 9、0.999 8、0.999 9、0.999 9);精密度、稳定性、重复性试验的RSD≤0.79%;尿嘧啶、尿苷、阿糖尿苷平均加样回收率为103.8%、102.2%、99.7%,RSD分别为2.44%、2.69%、3.16%(n=9)。结论:该方法准确、灵敏度高、专属性强、重复性好,可用于盐酸阿糖胞苷原料药的质量控制。     

HPLC法同时测定云连药材中6种生物碱的含量

目的:建立同时测定云连药材中6种生物碱含量的方法。方法:色谱柱为Xtimate～(TM)C_(18),流动相为30 mmol/L碳酸氢铵溶液(含0.1%三乙胺和0.7%氨水)-乙腈(梯度洗脱),流速为1.0 mL/min,检测波长为270 nm,柱温为30℃,进样量为10μL。结果:药根碱、非洲防己碱、表小檗碱、黄连碱、盐酸巴马汀、盐酸小檗碱的检测质量浓度线性范围分别为0.85～16.96 mg/L(r=0.999 9)、1.25～24.96 mg/L(r=0.999 8)、2.05～40.96 mg/L(r=0.999 9)、3.65～72.96 mg/L(r=0.999 9)、2.88～57.60 mg/L(r=0.999 9)、13.25～264.96 mg/L(r=0.999 9);精密度、稳定性、重复性试验的RSD<3.0%;加样回收率分别为97.14%～102.14%(RSD=1.93%,n=6)、97.00%～102.00%(RSD=2.06%,n=6)、98.18%～101.82%(RSD=1.79%,n=6)、96.15%～101.28%(RSD=2.06%,n=6)、96.88%～101.88%(RSD=1.87%,n=6)、99.31%～103.76%(RSD=1.89%,n=6)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于云连药材中6种生物碱含量的同时测定。     

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.     

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.

     

Lung disease and PKCs

The lung offers a rich opportunity for development of therapeutic strategies focused on isozymes of protein kinase C (PKCs). PKCs are important in many cellular responses in the lung, and existing therapies for pulmonary disorders are inadequate. The lung poses unique challenges as it interfaces with air and blood, contains a pulmonary and systemic circulation, and consists of many cell types. Key structures are bronchial and pulmonary vessels, branching airways, and distal air sacs defined by alveolar walls containing capillaries and interstitial space. The cellular composition of each vessel, airway, and alveolar wall is heterogeneous. Injurious environmental stimuli signal through PKCs and cause a variety of disorders. Edema formation and pulmonary hypertension (PHTN) result from derangements in endothelial, smooth muscle (SM), and/or adventitial fibroblast cell phenotype. Asthma, chronic obstructive pulmonary disease (COPD), and lung cancer are characterized by distinctive pathological changes in airway epithelial, SM, and mucous-generating cells. Acute and chronic pneumonitis and fibrosis occur in the alveolar space and interstitium with type 2 pneumocytes and interstitial fibroblasts/myofibroblasts playing a prominent role. At each site, inflammatory, immune, and vascular progenitor cells contribute to the injury and repair process. Many strategies have been used to investigate PKCs in lung injury. Isolated organ preparations and whole animal studies are powerful approaches especially when genetically engineered mice are used. More analysis of PKC isozymes in normal and diseased human lung tissue and cells is needed to complement this work. Since opposing or counter-regulatory effects of selected PKCs in the same cell or tissue have been found, it may be desirable to target more than one PKC isozyme and potentially in different directions. Because multiple signaling pathways contribute to the key cellular responses important in lung biology, therapeutic strategies targeting PKCs may be more effective if combined with inhibitors of other pathways for additive or synergistic effect. Mechanisms that regulate PKC activity, including phosphorylation and interaction with isozyme-specific binding proteins, are also potential therapeutic targets. Key isotypes of PKC involved in lung pathophysiology are summarized and current and evolving therapeutic approaches to target them are identified.     

Gender-related symptoms and correlates of alcohol dependence among men and women with a lifetime diagnosis of alcohol use disorders

This study explored gender-related symptoms and correlates of alcohol dependence in a crosssectional study of 150 men and 150 women with a lifetime diagnosis of alcohol use disorders (AUD). Participants were recruited in equal numbers from treatment settings, correctional centres and the general community. Standardized measures were used to determine participants' use of substances, history of psychiatric disorders and psychosocial stress, their sensation seeking and family history of substance use and mental health disorders. Multivariate analyses were used to detect patterns of variables associated with gender and the lifetime severity of AUD. Men had a longer history of severe AUD than women. Women had similar levels of alcohol dependence and medical and psychological sequelae as men, despite 6 fewer years of AUD. More women than men had a history of severe psychosocial stress, severe dependence on other substances and antecedent mental health problems, especially mood and anxiety disorders. There were differences in family history of alcohol-related problems approximating same-gender aggregation. The severity of a lifetime AUD was predicted by its earlier age at onset and the occurrence of other disorders, especially anxiety, among both men and women. The limitations in the generalizability of these findings due to sample idiosyncrasies are discussed.     

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.