用RP-HPLC法分析地尔硫在兔体内的药动学及组织分布

以尼群地平为内标，用反相高效液相色谱法（ＲＰ－ＨＰＬＣ）测定兔口服地尔硫后血浆和组织器官的药物浓度。药动学符合二房室模型。主要参数∶Ｔ１／２（α）＝０．５１ｈ，Ｔ１／２（β）＝６．１１ｈ，Ｔ１／２（ｋａ）＝０．２５ｈ，Ｔ（ｐ）＝０．５２ｈ，口服２ｈ后在胆汁、血、脾、心、肾、肝、大脑和小脑药物浓度分别为∶０．５５９ｍｇ／Ｌ、０．３７５ｍｇ／Ｌ、４．５６２μｇ／ｇ、０．７７１μｇ／ｇ、１．０９３μｇ／ｇ、１．４３９μｇ／ｇ、０．３５９μｇ／ｇ和０．７４１μｇ／ｇ。     

免疫抑制鼠肾包膜下法检测口腔颌面部恶性肿瘤联合化疗敏感性的实验研究

将18例口腔颌面部恶性肿瘤做原代移植物，移植到CTX免疫抑制鼠SRC，检测了联合化疗敏感性，结合病理学观察，结果：①以对照组△TS≥－0．5omu标准，获可评价率88％（16／18）；SRC移植瘤阳性生长81．2％（69／85），零生长7％（6／85），负性生长11．8％（10／85）。②以对照组与实验组△TS（P＜0．05），移植瘤消退率≥15％为标准，68．8％（11／16）可评价药物敏感性，对PM、PVF、CVP敏感率分别为54．5％（6／11）、60％（6／10）、63.6％（7／11）。病理学证实，对照组移植瘤名存良好，实验组移植瘤有不同程度的退行性改变。③Ag－NOR计数和DNA含量测定结果，化疗敏感组与对照组之间存在显著差异。证实CTX免疫抑制既SRCA对口腔颌面部部分恶性肿瘤实现个体化疗是一简便快速方法。     

对1973年一起周围神经病爆发的病因再认识──三邻甲苯磷酸酯引起的中毒事例

流行病学资料1973年6～7月，陕西省凤翔县石落务大队党家村2、3两个生产队在45天中爆发了多发性周围神经病患者34例。按2、3队人口计算，发病率分别为1．5％（3／197）和9．2％（31／338）。病因调查排除了营养缺乏、水源污染和其它可能的共同因素后，发现与3队春天向西秦大队一次“借粮”有关。3队36户借粮，8户发病；12户未借粮，无1例患者（P＝0．09）。在36个借粮户中，9户超借，5户发病（5／9）；未超偌27户，3户发病（3／27）（P＜0．01）。如按超猎户与未超猎户家庭人口计算发病串，超借户33．3％（20／60），来租借户5．6％（11／1…     

柠檬酸酸洗废液处理中活性污泥的培养与驯化

针对柠檬酸酸洗废液的处理，取大连开发区污水处理厂经脱水干化的活性污泥作种泥，将生活污水与柠檬酸废水以一定比例混合，进行污泥的培养与驯化．驯化中不断增加柠檬酸废水的比例，使CODcr从330mg／L逐渐上升到1982mg/L，在水温：20℃～25℃，溶解氧：4．0～5．0mg／L，pH值：6．5～8．0，SVI：30％左右，MLSS：2～4mg/L的条件下，经过7d的培养驯化，柠檬酸废液CODcr的去除率达到90％以上，15d，生物反应器中微生物繁殖良好，形成稳定的活性菌胶团絮体，结果表明：试验控制条件适宜，驯化好的活性污泥对柠檬酸酸洗废液中的有机物去除效果稳定，达到了预期的目的。     

直肠灌注安定溶液治疗小儿严重惊厥30例分析

用直肠灌注安定溶液的方法治疗30例严重惊厥患儿，按0．5mg／kg剂量单次给药后，21例惊厥在10min内停止，3例给予重复灌肠后1例惊厥停止。直肠给药后7～10min测定安定血清浓度为44～10．3ng／L，平均（6．9±2．6）ng／L。直肠灌注安定溶液是紧急治疗小儿严重惊厥安全有效的方法。     

新型聚硅酸氯化铝铁絮凝剂制备与性能

以水玻璃、氯化铝、氯化铁为原料制备新型无机絮凝剂——聚硅酸氯化铝铁,考察聚硅酸熟化时间、熟化温度、熟化pH、Al／Fe摩尔比等参数的影响．确定了最佳制备条件．同时,以生活污水为处理对象考察了pH、投药量对絮凝性能的影响．研究结果表明：当硅酸钠浓度为0．97mol／L,Si／（Al＋Fe）为2：（2＋1）、Al／Fe为2：1～4：1时,熟化温度30～40℃、pH为5～6、熟化时间20～30min的条件下,制备的聚硅酸氯化铝铁对于pH为6～11的生活污水的混凝处理效果最佳．采用相同投加量时,絮凝效果明显优于传统絮凝剂。     

子宫颈癌患者组织HPV16 E_6、E_7基因及其血清抗体检测

用多聚酶链反应检测子宫颈癌组织HPV16E6、E7基因，同时用基因工程方法制备E6、E7抗原，以免疫酶联吸附法检测其血清抗体。结果表明，宫颈癌组织中HPV16E6、E7DNA检出总阳性率为71．8％，E6、E7基因检出率分别为37．5％（12／32）和65．6％（21／32）。HPV16E6、E7血清抗体反应     

血清中普萘洛尔的固相萃取及荧光法测定

血清中的普萘洛尔经自制的硅胶固相萃取柱提取后，在水溶液中于岛津ＲＦ－５４０荧光分光光度计测定荧光强度（Ｅｘ２ｇ８ｎｍ、ＥＭ３４６ｎｍ、３ｎｍ／３ｎｍ、ＯＲ＝４）。当血清中普萘洛尔浓度在０．０３～０．７２ｍｇ／Ｌ范围内与荧光强度线性相关，回归方程Ｃ＝０．０２８５Ｆ－０．０７５、ｒ＝０．９９９７．血清中平均回收率为９８．３８＋３．８６（ＳＤ）％、ＣＶ＝３．９２％（ｎ＝１２）。用本文建立的方法测定了家兔灌胃给药后的血药浓度，并用ＭＣＰＫＰ药动学程序进行了药代动力学参数的计算。     

胃癌中内分泌细胞及其意义

应用免疫组化ABC法对48例胃癌进行胃泌素、生长抑素、胰高血糖素标记。结果胃泌素阳性14例（29．2％），生长抑素阳性9例（18．7％），两者均阳性者6例（12．5％）。未分化腺癌中内分泌细胞阳性率较高分化腺癌高。胃泌素阳性组其浆膜浸润率13／14例（92．9％），淋巴结转移率11／14例（78．5％），明显高于阴性组（P<0.01）。生长抑素阳性组浆膜浸润率6／9例（66．7％），淋巴结转移率4／9例（44．4％），与阴性组相比均无明显差异（P＞0．05），提示胃泌素有促进癌细胞生长的作用，癌细胞生长愈活跃，其侵袭能力愈强，转移率愈高。     

子宫颈癌患者组织HPV16 E_6、E_7基因及其血清抗体检测

用多聚酶链反应检测子宫颈癌组织HPV16E6、E7基因，同时用基因工程方法制备E6、E7抗原，以免疫酶联吸附法检测其血清抗体。结果表明，宫颈癌组织中HPV16E6、E7DNA检出总阳性率为71．8％，E6、E7基因检出率分别为37．5％（12／32）和65．6％（21／32）。HPV16E6、E7血清抗体反应阳性率为68．18％（30／44）和56．18％（25／44）。结果同时显示HPV16E6、E7DNA分布并不均一，存在E 6、E 7、E 6E 7和E6-E-74种模式，并且其血清抗体反应和DNA存在情况也不一致，E6抗体阳性的24例患者中，仅9例可检出其DNA，E，同样如此。这些似…     

HPLC法测定健宝胶囊中淫羊藿苷含量

目的　建立健宝胶囊中淫羊藿苷的含量测定方法。方法　采用高效液相色谱法 ,色谱柱为C18(15 0mm×4.6mm) ,流动相为乙腈 0 .0 75mol·L-1磷酸溶液 (2 5∶75 ) ,流速 1.0mL·min-1,检测波长为 2 70nm。结果　淫羊藿苷进样量在 0 .0 6～ 0 .30 μm范围内 ,线性关系良好 (r=0 .9991) ,方法回收率为 98.5 0 %(n =5 ,RSD =1.2 0 %)。结论　本方法准确、简便、快速 ,适合于该药的质量分析检验。     

家兔生殖腺及三阴交穴区的传入神经的节段性分布——HRP法及荧光双标法研究

本实验用HRP、EB、TY三种不同浓度水溶液, 注入成年家兔生殖腺浆膜下和三阴交穴区。HRP、EB、TY借内脏与躯体传入神经的摄取和逆行传送;用~3H—亮氨酸注入成年猫胸腰段脊神经节,借顺行传送来验证。用上述三种方法追踪在脊神经节中显示了生殖腺与三阴交穴区传入神经起源的胞体及节段性分布,观察到二者在脊神经节的重合区。结果表明:1.睾丸的传入神经的标记细胞多分布于脊神经节T_(11)～L_4。2.卵巢的传入神经的标记细胞多分布于T_(10)—L_4。3.三阴交穴区的传入神经的标记细胞多分布于L_4～S_3。4.生殖腺与三阴交穴区的传入神经标记细胞在脊神经节的重合区为T_7～L_7。另外,对HRP法、荧光双标记法、ARG法的应用,一些内脏器官与体表穴区的传入神经的节段性及其重合区进行了讨论。     

用薄层色谱法测定骨康片中士的宁和马钱子碱含量

目的 建立骨康片中士的宁和马钱子碱的含量测定方法。方法 采用双波长薄层扫描法，硅胶GF２５４薄层板，展开剂为甲苯丙酮乙醇浓氨试液(4∶3∶1∶2)，检测波长，士的宁λＳ＝２５８nｍ，λＲ＝３１０ｎｍ；马钱子碱λＳ＝３０１ｎｍ，λＲ＝３３５ｎｍ。结果 士的宁和马钱子碱的相关系数分别为0..9996和0..9999，方法的回收率分别为99..83%(RSD=1.03%)和96..09%(RSD=2.01%)。结论 方法准确、简便、重现性好，同时可以定量测定骨康片中士的宁和马钱子碱含量，可作为该药的质量控制方法。     

葛根中有效部位及有效成分的高效液相色谱分析

目的建立全面控制葛根及其制剂的定性和定量分析方法。方法用反相高效液相色谱法(RPHPLC),以甲醇水(42∶58)为流动相在250nm波长下检测,对葛根有效部位(醋酸乙酯提取部位)进行指纹图谱定性分析,对葛根有效部位中的有效成分葛根素和大豆苷元进行定量测定,并对11种不同来源的葛根药材进行分析测定。结果在定性分析条件下,葛根有效部位的HPLC指纹图谱中有5个共有峰,可以作为其定性鉴别的指标峰;在以葛根素和大豆苷元为定量指标分析中,其方法的回收率分别为98.0%和95.4%,相对标准偏差(RSD)分别为1.30%和1.61%,葛根药材中葛根素和大豆苷元的含量分别在0.213%～3.626%和0.012%～0.049%范围内。结论以葛根有效部位指纹图谱定性分析和有效成分定量分析方法,可以准确有效地控制其质量。     

Rapid quantification of the metabolite of valacyclovir hydrochloride in human plasma by liquid chromatography-tandem mass spectrometry

Objective To establish a rapid, sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of acyclovir (the metabolite of valacyclovir hydrochloride) in human plasma. Methods After addition of ganciclovir as internal standard (IS), plasma samples were prepared by one-step protein precipitation using acetonitrile as precipitant, followed by an isocratic elution with 0.1% formic acid 3.5μm) column. Detection was performed on a triple-quadrupole mass spectrometer utilizing electrospray ionization (ESI) interface operating in positive ion and selected reaction monitoring (SRM) mode with the precursor to product ion transitions m/z 226.2→152.1 for acyclovir and m/z 256.2→152.1 for the IS. Results The analytical results demonstrated a good linearity over the ranges from 0.005 to 4μg/mL (r=0.9999) for valacyclovir hydrochloride. The relative standard deviations (RSD) of intra-batch and inter-batch were less than 4.06% and 9.23%, respectively. The limit of detection and lower limit of quantification in human plasma were 2ng/mL and 5ng/mL, respectively. Conclusion The method was simple, sensitive, accurate and reproducible and has been successfully applied to a bioequivalence study of valacyclovir hydrochloride capsules in Chinese healthy male volunteers.     

RP-HPLC method for the quantitation of β-Sitosterol in Elaeagnus Gon yanthes Benth

Objective To establish an RP-HPLC method for the determination of β-Sitosterol in Elaeagnus Gonyanthes Benth. Methods The separation was performed on a luna C8 (2) (150 mm×4.6 mm, 5μm) column with the mobile phase of methanol-water (88∶12, v/v) at a flow rate of 1.0 mL/min, the detection wavelength was set at 210 nm, and the temperature of the column was maintained at 35 ℃. Results The calibration curve of β-Sitosterol was linear over the concentration range of 0.075-0.375 mg/mL (r=0.9999) and the average recovery of β-Sitosterol was 96.30% with RSD of 3.60%(n=3). Conclusion The method is simple, rapid, and accurate, and can be used for the quality control of Elaeagnus Gonyanthes Benth.     

Analysis of ganciclovir and its related substances using high performance liquid chromatography and liquid chromatography-mass spectrometry methods

Objective High performance liquid chromatography (HPLC) and liquid chromatography-mass spectrometry (LC/MS) methods were developed for the determination of ganciclovir and its related substances. Methods A Hypersil ODS2 column (4.6mm×250mm, 5μm) was used with a mobile phase of 0.02M potassium 1.0mL/min, and UV detector set at 254nm was used for monitoring the eluents. Results The method was simple, rapid, selective and capable of separating all related substances at trace level with a detection limit of 0.04μg/mL. It has been validated with respect to accuracy, precision, linearity, and limits of detection and quantification. The linearity range was 10.2-153.0μg/mL with r=0.9998. The percentage recoveries ranged from 96.7% to 101.6%, and RSD was 1.24%-1.96% (n=5). Conclusion The method was found to be suitable not only for monitoring the reactions during the process development but also for quality control of ganciclovir. For identification of related substances, LC/MS was used. The mainly related substances of ganciclovir active pharmaceutical ingredients (API) were determined as guanine, (1, 3-dioxolan-4-yl) methyl acetate, and diacetyl guanine.     

LC-ESI-MS/MS, a modified method for simultaneous quantification of isoflavonoids, flavonoids, alkaloids and saponins in a Chinese herbal preparation Gegen-Qinlian decoction

A sensitive and reliable liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS) method was established to simultaneously quantitate four categories of compounds (isoflavonoids, flavonoids, alkaloids and saponins) in Gegen-Qinlian decoction (GQD). These compounds were separated by a Shiseido CAPCELL PAK C18 column with a linear gradient consisting of 0.1% (v/v) formic acid in water (A) and 0.1% (v/v) formic acid in acetonitrile (B), and delivered at a flow rate of 0.3 mL/min. All the analytes were determined by electrospray positive ionization tandem mass spectrometry in a multiple reaction monitoring (MRM) mode. Linearity, accuracy, precision, recovery and stability of the method were evaluated with the validation over the range of 4.0-538 5 ng/mL. The proposed method was applied to the analysis of a Chinese herbal preparation GQD successfully.     

A rapid method for the determination of dopamine in porcine muscle by pre-column derivatization and HPLC with fluorescence detection

A rapid method has been developed based on the sample preparation procedure named as QuEChERS （Quick, Easy, Cheap, Effective, Rugged and Safe）, combined with reversed-phase high performance liquid chromatography with fluorescence detector and C18 column after precolumn derivatization using o-phthalaldehyde and 2-mercaptoethanol to determine dopamine in porcine muscle. Methanol and deionized water （0.1% acetic acid, v/v） with a ratio of 60：40 was used as mobile phase. The flow rate was 0.8 mL/min and dopamine was eluted within 15 min. The linearity range was 0.003-8 μg/mL with r=0.9992. The detection limit for dopamine was 4 μg/kg and the quantification limit was 9 μg/kg. Recovery studies were carried out at 0.1, 0.5 and 1.0 mg/kg fortification levels and the average recoveries obtained ranged from 90.4% to 98.2% with relative standard deviations between 3.5% and 8.1%. The method was found to be suitable for detection of dopamine in animal product tissues at the maximum residue level.