反相高效液相色谱法测定猪脑提取物中神经生长因子的含量

目的 建立猪脑提取物中神经生长因子含量测定的方法。方法 采用高效液相色谱法,色谱柱为Dia monsil C18(150 mm×4.6 mm,5 μm),流动相为乙腈:(0.5％三氟乙酸水溶液:甲醇=52:48)=30:70,10 min后 梯度升至50:50。柱温30℃,流速1.0 mL／min,波长280 nin,进样量20μL。标准曲线法计算含量。结果 在 该色谱条件下,测得神经生长因子的线性良好(r=0.999 4);平均回收率100.9％-102.4％;日内精密度RSD 1.36％-1.77％,日间精密度RSD 1.85％-2.40％;最低检测浓度0.25 mg／L;3批样品中神经生长因子含量分 别为0.326％、0.321％0.332％(mg／100 g)。结论 该方法灵敏、准确、可靠,适用于本品中神经生长因子含量的 测定。     

Obtaining a highly purified preparation of class I HLA antigens

Institute of Molecular Biology, Academy of Sciences of the USSR. Institute of Carcinogenesis, All-Union Oncologic Scientific Center, Academy of Medical Sciences of the USSR, Moscow. (Presented by Academician of the Academy of Medical Sciences of the USSR N. N. Trapeznikov.) Translated from Byulleten' Éksperimental'noi Biologii i Meditsiny, Vol. 110, No. 10, pp. 401–402, October, 1990.     

5-氟尿嘧啶毫微囊的药物动力学研究

本文报告了5-氟尿嘧啶毫微型胶囊(5-Fu NC)的药物动力学研究结果:兔体内单次静注给药后,用高效液相色谱法测定了5-Fu Nc和5-氟尿嘧啶注射液的血药浓度,并且用PKBPN1药代程序计算了各项药物动力学参数。结果表明:制成毫微囊后,5-氟尿嘧啶在体内分布得更为迅速,作用时间也更长。     

气相色谱法测定黄柏果挥发油中β-香叶烯含量

本文报道了用气相色谱法制备β-香叶烯纯品,用程序升温气相色谱法测定黄柏果挥发油中β-香叶烯含量,用标准曲线法定量。线性范围为0～0.5mg/ml,回收率为99.0%,变异系数小于1%.本法可用于喘复康胶丸及原料油的质量鉴定。     

维C银翘片中对乙酰氨基酚含量测定方法改进

目的:采用高效液相色谱法(HPLC)测定维C银翘片中对乙酰氨基酚的含量,以避免用双波长分光光度法测定时出现的干扰因素.方法:采用HPLC法,双波长分光光度法分别测定不同批号的维C银翘片中对乙酰氨基酚的含量.结果:双波长分光光度法较繁琐、误差大,HPLC法简便、快速、准确.结论:HPLC法准确可靠,适用于维C银翘片的质量控制.     

高效液相色谱法测定十全大补丸中芍药苷的含量

目的:采用高效液相色谱法测定十全大补丸中芍药苷的含量,以控制该制剂的质量.方法:以C18化学键合硅胶柱分离芍药苷,以乙腈 0.1%磷酸(15∶85)为流动相,UV检测波长230 nm进行测定.结果:芍药苷峰与其他组分峰的分离度为3.9,理论塔板数以芍药苷峰计算为35 440;方法的平均加样回收率99.0%(n＝5);5次独立测定的相对偏差RSD＝0.90%,芍药苷在0.25～2.50 μg范围内,浓度与吸收面积值呈良好的线性关系.结论:本法测定十全大补丸中芍药苷的含量,结果准确,重复性好.     

超临界流体色谱及其应用

介绍了超临界流体的特性,超临界流体色谱(SFC)的概念及其发展。讨论了SFC的设备以及SFC/FTIR,SFC/MS的联用技术,并与经典的色谱法GC和HPLC进行了对照。对其在药物分析中的应用作了介绍。     

气相色谱分析法测定酸奶和奶油中c9,t11-共轭亚油酸的含量

目的：建立用程序升温气相色谱法测定奶制品中c9,t11-共轭亚油酸含量的方法。方法：首先建立本实验方法的气相色谱分析条件；采用内标法，将样品提取、甲酯化后，进行气相色谱分析；同时对实验方法的回收率、精密度也进行了分析。结果：能够将甲酯化亚油酸和c9,t11-共轭亚油酸很好地分离；内标物十七烷酸甲酯与其它脂肪酸甲酯能够完全分离，并不受样品中其它组分的影响；c9,t11-共轭亚油酸的含量分别为：帕玛拉特天然酸奶饮品10．78mg/g，万家宝原味酸奶（搅拌型）5．03mg/g，奶油22．54mg/g脂肪。实验方法的回收率为84．74％，RSD＝3．73％；精密度RSD＝2．58％。结论：所建立的实验条件准确可靠，这对于分析奶及奶制品来源的c9,t11-共轭亚油酸含量具有指导意义。     

兔体内乌头碱代谢产物研究

目的鉴定乌头碱在家兔尿中主要代谢产物。方法ig给药(5 mg·kg^-1)后,收集给药后♂家兔尿液,固相萃取柱富集、液相色谱-电喷雾离子阱质谱法分离鉴定乌头碱代谢物。结果在给药后尿样中发现乌头碱原形和4种代谢物M1～M4,分别测得准分子离子峰［M+H］+及其各级碎片离子。结论M1～M4为乌头碱的4个代谢物,推测分别为16-O-去甲基乌头碱、乌头次碱、16-O-去甲基乌头次碱、乌头原碱。     

In vitro metabolism of a nitroderivative of acetylsalicylic acid (NCX4016) by rat liver: LC and LC–MS studies

The metabolism of a nitroderivative of acetylsalicylic acid, benzoic acid, 2-(acetyloxy)-3-[(nitrooxy)methyl]phenyl ester (NCX4016), the lead compound of a new class of NO-releasing non steroidal-antiinflammatory drugs has been studied in vitro in rat liver subcellular fractions (S 9000×g, microsomes, cytosol). Samples were extracted with CH₃CN (2 vol.) containing 1% H₃PO₄ (2 M), vortexed for 3 min and then centrifuged for 5 min at 5000 rpm. Supernatants were diluted with 0.02 M phosphoric acid and analysed by reverse-phase LC. Linearity of calibration for NCX4016 and metabolites was observed over the range 0.25–50 μg/ml with coefficients of determination greater than 0.9996. Extraction efficiency from spiked liver samples ranged from 85 to 95% for all the analytes. In the S 9000×g fraction, NCX4016 undergoes rapid metabolization, with the formation of salicylic acid (SA) and [3-(nitrooxymethyl)phenol] (HBN). HBN is then rapidly metabolised to 3-hydroxybenzylalcohol (HBA), and mainly to a new metabolic species, whose formation takes place specifically in the liver cell cytosol. LC–MS analysis (electrospray ionisation) of the cytosol extract in negative and positive-ion modes furnished deprotonated [M−H]⁻ and protonated [M+H]⁺ molecular ions at m/z 412 and 414, respectively, accompanied by the typical clusters with sodium. MS/MS analysis in negative-ion mode, by selection and collision of the ion at m/z 412, gave a fragmentation pattern characterized by the ions at m/z 272 and 254, which allowed to assign the structure of 1-(glutathion-S-yl)methylene-3-hydroxy-benzene, a conjugated product between GSH and the benzyl carbon atom of HBN. In rat liver cytosol HBN is completely metabolised to this thioether adduct within 30 min incubation; the process is enzymatically mediated by GSH transferase and strictly dependent on GSH availability. The relevance of this new metabolic pathway in NCX4016 detoxification by rat liver is discussed.