毛细管气相色谱法测定联苯双酯有机溶剂的残留量

目的建立气相色谱法测定联苯双酯中3种有机溶剂的残留量的方法。方法采用DB-624毛细管色谱柱（30.0m×0.53mm×3μm）;进样口温度为200℃;FID检测器温度为260℃;柱温：程序升温,60℃保持5min,然后以20℃/min的速率升温220℃,保持5min;以氮气为载气,恒压模式,载气压力为2.4psi;直接进样,进样量为1μL;以二甲基亚砜为溶解介质,测定了联苯双酯中乙醇、二氯甲烷和N,N-二甲基甲酰胺的残留量。结果乙醇、二氯甲烷和N,N-二甲基甲酰胺及溶剂峰彼此均能良好分离,线性范围分别为0.90～401.72μg·mL-1（r=0.9999）,2.51～50.20μg·mL-1（r=0.9999）,1.43～75.36μg·mL-1（r=0.9998）;方法重复性良好,回收率也符合规定。结论该法适用于联苯双酯中这3种有机溶剂残留量的测定。     

顶空气相色谱法测定盐酸克林霉素中的残留溶剂

目的：建立顶空毛细管气相色谱法测定盐酸克林霉素中有机溶剂残留量。方法：采用顶空气相色谱法,色谱柱为DB-624毛细管柱,载气为氮气,流速为2 ml·min^-1,分流比为1∶1。 FID检测器,检测器温度为300℃;进样口温度为200℃;柱温采取程序升温,起始温度40℃,保持5 min,以20℃·min^-1升温至200℃,持续10 min。顶空进样,平衡温度为80℃,平衡时间为30 min。以水为溶剂,外标法测定盐酸克林霉素中甲醇,乙醇,丙酮,三氯甲烷和N,N-二甲基甲酰胺的残留量。结果：在此色谱条件下,各有机溶剂均能得到有效分离,在所考察的浓度范围内线性关系良好,r=0.9991~0.9999;平均回收率为97.2%~101.2%,RSD为0.68%~1.98%（n=9）。结论：本试验建立的顶空气相色谱方法适合盐酸克林霉素原料中有机溶剂残留量的检测。     

毛细管气相色谱法测定达沙替尼原料药中6种残留溶剂

目的：建立毛细管气相色谱测定达沙替尼原料药中吡啶、二氯甲烷、甲醇、N,N-二甲基甲酰胺、二甲亚砜、乙醇6种有机溶剂残留量的方法。方法采用DB-624(30 m×0.53 mm,3μm)毛细管柱;氢火焰离子化检测器;程序升温：初始温度25℃(维持13 min),再以15℃·min-1升至150℃(维持5 min),再以40℃·min-1升至220℃(维持5 min);载气为氮气;柱流速为2.0 mL·min-1;进样口温度：230℃;检测器温度：250℃;分流直接进样,以N,N-二甲基乙酰胺为溶剂,进样体积为0.5μL。结果6组分均能良好分离,6组分峰面积与浓度均呈良好的线性关系,其中吡啶、二氯甲烷、甲醇、N,N-二甲基甲酰胺、二甲亚砜、乙醇的线性范围分别为4.16~31.21μg·mL-1(r=0.9998),12.12~90.92μg·mL-1(r=0.9994),59.98~449.85μg·mL-1(r=0.9998),18.16~136.19μg·mL-1(r=0.9993),100.25~751.86μg·mL-1(r=0.9991),100.30~752.28μg·mL-1(r=0.9999),平均回收率为98.4％~101.3％(RSD=2.8％~5.0％)。结论该方法简单、灵敏、准确,可用于测定达沙替尼原料药中的残留溶剂。     

盐酸法舒地尔残留溶剂检查的方法学研究

目的建立测定盐酸法舒地尔中有机残留溶剂的顶空气相色谱法。方法采用顶空气相色谱法,DB-624柱(6%氰丙基苯基-94%二甲基聚硅氧)(30 m×0.25 mm×1.4μm),氢离子火焰检测器(FID),程序升温,载气为氮气,进样口温度为200℃,检测器温度为250℃。结果四种有机溶剂甲醇、乙醚、二氯甲烷和N,N-二甲基甲酰胺完全分离,在所考察的浓度范围内具有良好线性,相关系数均在0.998以上,甲醇、乙醚、二氯甲烷和N,N-二甲基甲酰胺的最低检出浓度分别为3.057μg.mL-1、0.020μg.mL-1、1.313μg.mL-1、8.184μg.mL-1,平均回收率为100.52%、100.82%、101.14%、100.62%。结论本方法简便,准确,灵敏,适用于盐酸法舒地尔中有机残留溶剂的测定。     

GC测定盐酸伊达比星原料药中的残留溶剂

目的建立盐酸伊达比星原料药中残留溶剂的检查方法。方法采用毛细管色谱柱顶空进样气相色谱程序升温法测定。色谱柱为DB-624石英毛细管柱（30．0m×0．530mm,3．00μm）;进样口温度：200℃;氢火焰离子化检测器（FID）温度：250℃;柱温：程序升温,初始温度50℃,保持6min,再以10℃·min叫的升温速率升至165℃,维持2．5min;载气：氮气;流速：4．0mL·min^-1。顶空进样,平衡温度：105℃,平衡时间：20min,进样体积：1．0mL。以二甲基甲酰胺（DMFl为溶解介质。结果各被测溶剂均能良好分离,各溶剂峰面积与浓度均呈良好的线性关系,方法的精密度良好,各溶剂的回收率较为理想。结论该法适用于盐酸伊达比星原料药的残留溶剂测定。     

盐酸头孢吡肟中N-甲基吡咯烷的气相色谱测定法

目的:建立用气相色谱的顶空进样法测定盐酸头孢吡肟中N-甲基吡咯烷残留量。方法:用HP-5,0.53 mm×30 m色谱柱,以氮气为载气,FID检测器,顶空进样,通过外标法计算盐酸头孢吡肟中N-甲基吡咯烷的残留量。结果:盐酸头孢吡肟中检出N-甲基吡咯烷,标准曲线的线性范围为43.4-347.2μg·mL-1,相关系数为0.9997;定量限为4.17μg·mL-1;平均加样回收率为98.8％,RSD为2.8％。结论:本法快速、简便,灵敏度高,分离度好。     

顶空毛细管气相色谱法测定头孢克肟颗粒中乙醇残留量

目的:建立顶空毛细管气相色谱法测定头孢克肟颗粒剂中的乙醇残留量分析方法。方法:采用顶空进样气相色谱法,以丙酮为内标,键合聚乙二醇（HP-INNOWAX）石英毛细管色谱柱;柱升温程序:50℃（保持6 min）,以40℃·min^-1的速率升至150℃（保持5 min）;进样口温度200℃;检测口（FID）温度250℃;氮气为载气,流速:1.0 ml·min^-1;分流进样,分流比1.0:1;顶空温度85℃,平衡时间30 min,进样时间1 min。结果:乙醇在0.02～1.00 mg·nl^-1浓度范围内线性关系良好,r=0.999 7,最低检测限为0.1μg·ml^-1。加样回收率为86.8%,RSD=1.96%。结论:本法简便、快速、结果准确,适用于头孢克肟颗粒剂中乙醇残留量检测。     

顶空气相色谱法测定盐酸倍他洛尔中6种有机溶剂残留量

目的建立气相色谱法测定盐酸倍他洛尔中丙酮、乙酸乙酯、异丙醇、乙腈、甲苯、N,N-二甲基甲酰胺6种有机溶剂残留量。方法采用气相色谱法,色谱柱为DB-WAX石英毛细管柱(30.0m×0.53mm,1.0μm),载气为氮气,进样口温度为250℃,FID检测器温度为280℃;柱温为50℃,保持5min,以15℃·min-1升温速率升至200℃,维持6min,溶剂为二甲基亚砜。结果被测物均能得到很好的分离,峰面积与质量浓度线性关系良好,精密度和回收率良好。结论该方法准确、可行,可作为盐酸倍他洛尔的质量控制与评价的一种直观、合理、有效的技术手段。     

顶空气相色谱法测定醋酸奥曲肽原料中的残留溶剂

目的：采用顶空气相色谱法测定醋酸奥曲肽原料中的残留溶剂。方法：采用6%腈丙基苯基-94%二甲基聚硅氧烷(DB-624)毛细管色谱柱(30 m×0.32 mm×0.25 μm),柱温为程序升温：初始温度为40 ℃,保持4 min,然后以20 ℃?min-1的升温速率升至200 ℃,保持15 min,进样口温度200 ℃,氢火焰离子化检测器,检测器温度280 ℃,分流比2:1,载气流速为1.0 mL?min-1。结果：4种残留溶剂均能完全分离,甲醇、乙腈、二氯甲烷、N,N-二甲基甲酰胺线性范围分别为19.89～318.18mg?mL-1 (r=0.999 7)、4.19～67.07mg?mL-1 (r=0.999 7)、11.69～58.44mg?mL-1 (r=0.999 7)和20.38～122.28mg?mL-1 (r=0.999 7);检测限分别为1.30、0.03、0.02μg和3.76μg。结论：该方法重复性好,灵敏度高,可用于醋酸奥曲肽原料中的残留溶剂控制。     

顶空气相色谱法测定溴吡斯的明原料药中的残留溶剂

目的采用顶空气相色谱法测定溴吡斯的明原料药中的残留溶剂。方法色谱柱为PEG-20M(38 mm×0.25mm,0.32μm),氢火焰离子化检测器,载气为氮气,进样口温度为200℃,检测器温度为250℃。柱温为程序升温:初始温度50℃,保持5 min,再以10℃.min-1的速率升温至150℃,保持5 min,顶空条件:顶空平衡温度80℃,平衡时间30 min。结果该方法中溴吡斯的明的残留溶剂得到了较好的分离与测定。丙酮在0.25~0.75 mg.mL-1,乙醇在0.25~0.75 mg.mL-1,甲苯在0.044 5~0.133 5 mg.mL1线性关系良好,相关系数分别为0.999 2、0.998 2、0.995 6。丙酮、乙醇和甲苯的精密度(RSD)分别为3.2%、2.8%、4.1%(n=6),回收率分别为100.5%(RSD=4.6%)、98.4%(RSD=5.5%)和101.2%(RSD=3.7%)(n=6)。结论该方法可用于溴吡斯的明原料药中的残留溶剂测定。     

Optimizing [13N]N2 radiochemistry for nitrogen‐fixation in root nodules of legumes

Here we explored the conditions for synthesizing [¹³N]N₂ in a state that is suitable for the administration to plant root nodules enabling studies of nitrogen fixation. [¹³N]N₂ was prepared batchwise, starting with [¹³N]NO from the ¹⁶O(p,α)¹³N nuclear reaction on a liquid water target. [¹³N]NO was first reduced to [¹³N]NH₃ using Devarda's alloy, and then the [¹³N]NH₃ was oxidized to [¹³N]N₂ by hypobromite using carrier‐added NH₄Cl. The amounts of carrier NH₄Cl and hypobromite were varied to determine the effects these parameters had on the radiochemical yield, and on the radiotracer specific activity. As expected, increasing the amount of carrier NH₄Cl improved the radiochemical yield. Unexpectedly, increasing the amount of excess hypobromite from 1.6‐fold to 6‐fold molar equivalents (relative to NH₄Cl) improved the radiochemical yield and radiotracer specific activity under all conditions of carrier NH₄Cl. As a comparison, we measured [¹³N]N₂ specific activity derived from in‐target production based on a 50 µA min irradiation driving the ¹⁴N(p,pn)¹³N reaction on a gaseous N₂ target. The ‘wet’ radiochemistry approach afforded two advantages over the in‐target approach with a ～600‐fold improvement in specific activity, and the ability to collect the tracer in a small volume of gas (～20 mL at STP). Copyright © 2010 John Wiley & Sons, Ltd.     

One‐pot radiosynthesis of [13N]urea and [13N]carbamate using no‐carrier‐added [13N]NH3

The aim of this study was to develop a practical labeling method of [¹³N]ligands using no‐carrier‐added [¹³N]NH₃ with high specific activity. [¹³N]urea analogues [¹³N]1a and [¹³N]2a or [¹³N]carbamate [¹³N]3a were synthesized by reacting isocyanate 5a, carbamoyl chloride 6a or chloroformate 7a with [¹³N]NH₃. The precursors 5a–7a were prepared by treating amines 8a and 9a and alcohol 10a with triphosgene in situ. These reaction mixtures were not purified and were used directly for [¹³N]ammonolysis, respectively. Using the one‐pot method, we synthesized [¹³N]carbamazepine ([¹³N]4), a putative positron emission tomography ligand for brain imaging. Copyright © 2009 John Wiley & Sons, Ltd.     

N,N-二异丙基乙二胺的合成

目的合成得到N,N-二异丙基乙二胺,以降低生产成本。方法以二异丙胺和丙烯酰胺为起始原料,经Michael加成和Hofmann降解两步反应合成得到目标化合物。结果目标化合物总收率为55.3%,经核磁共振氢谱确证结构正确。结论该方法操作简单,原料廉价易得,适合工业化生产。     

N,N-dichlorotaurine: chemical and bactericidal properties

The biogenous antimicrobial agent N-chlorotaurine (NCT) converts by disproportionation to N,N-dichlorotaurine (NDCT) at a rate proportional to acidity. This occurs at appreciable amounts already in weakly acidic biological systems. To understand the consequences of NDCT formation, a thorough investigation of this undescribed compound was mandatory, which needed its synthesis. Differently from NCT, this was possible in the aqueous system using trichloroisocyanuric acid. While the free acid, Cl(2)HNCH(2)CH(2)SO(3)H, was not available in pure form, its sodium and potassium salts were analytically pure and showed melting points (decomposition) of 125-128 degrees C (potassium) and 162-164 degrees C (sodium). The sodium salt demonstrated unexpected long-term stability even at room temperature (8.4 % loss of activity within 4 months). The aqueous solutions of both salts exhibited a weak acid reaction, and they were less stable than NCT. With regard to chlorination of amines (transhalogenation), NDCT was, surprisingly, less efficacious than NCT, which manifested itself by a lack of reactivity at pH < 7, for which a mechanistic explanation is given. Compared on a molar scale, NDCT was more bactericidal than NCT against the gram-negative bacteria E. coli, P. aeruginosa and P. mirabilis, while there was no difference concerning the gram-positive ones, S. aureus and S. epidermidis. The increase of bactericidal activity at acidic pH was the same as observed with NCT and is attributed to a higher susceptibility of bacteria in this environment. Taken together, NDCT seems not to be suited to substitute NCT as a preparation fit for medical practice.     

单二乙氨基丙胺棉酚的合成及口服抗生育活性研究

单二乙氨基丙胺棉酚的合成及口服抗生育活性研究孔爱华１）朱崇泉薛慧中吴国沛（南京药物研究所，南京２１０００９）茅百勇赵世兴顾芝萍（上海药物研究所，上海２０００３１）在改变棉酚单个基团的结构改造工作中，作者先后合成了单甲氧基棉酚〔１〕、单醛棉酚和单苯胺棉...     

Flavin-containing monooxygenase 1-catalysed N,N-dimethylamphetamine N-oxidation

N,N-dimethylamphetamine (DMA) is a methamphetamine analogue known to be a weaker central nervous system stimulant than methamphetamine. Although a major metabolite of DMA is known to be DMA N-oxide (DMANO), which may be catalysed by flavin-containing monooxygenase (FMO), the specific enzyme(s) involved in this biotransformation has not been identified. In this study, the specific enzyme(s) involved with DMA N-oxidation was characterized by several assays. When DMA was incubated with different human recombinant drug-metabolizing enzymes, including FMOs and cytochrome P450s (CYPs), the formation of DMANO by FMO1 was the most predominant. The Michaelis–Menten kinetic constants for DMA N-oxidation by FMO1 were: K_m of 44.5 μM, V_max of 7.59 nmol min^?1 mg^?1 protein, and intrinsic clearance of 171 μl min^?1 mg^?1 protein, which was about twelve-fold higher than that by FMO3. Imipramine, an FMO1-specific inhibitor, selectively inhibited DMA N-oxidation. The resulting data showed that DMA N-oxidation is mainly mediated by FMO1.     

Possible mechanisms of controlling the configuration,stability, and lipophilicity of [99mTcO]N3S and [ReO]N3S chelates

The relationship of structural characters of the tripeptidic amine–bisamido‐thiol (N₃S type) chelators with the lipophilicity, configuration, and stability of four [^99mTcO]N₃S and one [ReO]N₃S chelates is studied here. The results show that the hydroxymethyl group on the two N₃S chelators, RP294 and RP435, has inhibited neither the formation nor interconversion of syn and anti stereoisomers of the chelates, while the tert‐butyl group on RP455 and RP535 has prevented the anti isomer from converting to the syn one both in acidic and neutral solutions. The interconversion rates of a stereoisomer can be accelerated at higher pH. [^99mTcO]RP455 is stable in pH 7.4 aqueous solution, while [^99mTcO]RP535 undergoes decomposition at the same medium, suggesting the influence of a larger side‐chain on the stability of the chelate. Unlike [^99mTcO]RP535, [ReO]RP535 is stable even in 0.1 N NaOH for 3 h without change. Combining factors of medium pH values, nature of substituents on a chelator's backbone, size of side‐chains, and property of central metal ions together determine the lipophilicity, configuration, and stability of [^99mTcO]N₃S and [ReO]N₃S chelates. This information may be useful for a further design of [^99mTcO]N₃S or [¹⁸⁶ReO]N₃S or [¹⁸⁸ReO]N₃S chelates with predictable physicochemical properties favorable for the quality diagnosis of cancers. Copyright © 2008 John Wiley & Sons, Ltd.     

氨氯吡咪及其衍生物DMA对豚鼠心肌细胞跨膜动作电位时程的影响

目的 :研究氨氯吡咪 (AM)及其衍生物二甲基氨氯吡咪 (DMA)对心室肌细胞跨膜动作电位时程(APD)的影响。方法 :利用全细胞膜片钳技术 ,观察 AM及其衍生物 DMA对豚鼠心肌细胞跨膜 APD的作用。结果 :Am可使 APD复极化 3 0 %、5 0 %和 90 %的时程 (APD3 0 ,APD50 ,APD90 )延长 3 0 %、5 2 %和 3 4%。 DMA可使APD复极化 APD3 0 、APD50 、APD90 的时程缩短 4 0 %、2 9%和 2 4 %。结论 :AM可使心肌细胞跨膜 APD延长 ,而DMA可使心肌细胞跨膜 APD缩短     

超声导向经皮置管引流治疗胰腺假性囊肿

超声导向经皮置管引流治疗胰腺假性囊肿山西医学院第二附属医院（０３０００１）阎汝川，任国良山西省儿童医院张玉新自１９８６年以来，我们采用Ｂ超引导经皮置管引流治疗胰腺假性囊肿１５例，全部治愈。现报道并讨论如临床资料１５例中，男６例，女９例：年龄最小者１９岁，最大者７５岁，平均４３岁。囊肿诱发原因：胰腺炎８例，腹部外伤７例。入院时均有上腹部疼痛，摸到肿块。其中７例有发热及呕吐，８例有血尿淀粉酶及白细胞计数增高。１５例经８超检查均提示为胰腺假性囊肿，肿块在胰体尾部９例，胰尾部６例，囊肿最大直径１３．２厘米，最小直径为５．９厘米。其中５例行ＣＴ检查，诊断均与Ｂ超检查相同。病人取仰卧位，全部应用Ｂ超定位，确定囊肿位置及穿刺点。测量皮肤至囊肿的最近距离，并避开腹内脏器和大血管。消毒皮肤及铺无菌孔单，１％的普鲁卡因局部浸润麻醉，用２２号带针蕊的ＰＴＣ针（外径０．７ｍｍ，内径０．５ｍｍ）穿刺进入囊腔，拔去针蕊，接注射器抽取少量囊液证实确为囊肿，并同时将抽出液送生化、常规、细胞学及细菌学检查。然后更换腹腔套管针。拔出ＰＴＣ针，在原穿刺点切开皮肤，刺入腹腔套管针，置管行外引流术。１５例均一次穿刺置管成功。其中一例在引流期间自行脱     

~(99m)Tc-MIBI心肌断层显像和动态心电图对冠心病的对比观察

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