凝胶渗透色谱-液相色谱法测定沉积物中多环芳烃的不确定度评定

目的 对凝胶渗透色谱-液相色谱法测定沉积物中多环芳烃不确定度进行评定。分析不确定度来源,计算各不确定分量,以控制测定结果准确度。 方法 依据JJF 1059.1-2012 《测量不确定度评定与表示》和CNAS-GL06-2006 《化学分析中不确定度的评估指南》中有关规定,从标准溶液配制,样品前处理,仪器测定重复性等方面对测定结果的不确定来源进行评定。 结果 评定结果显示标准曲线,仪器测定的重复性和样品前处理是不确定度的主要来源。 结论 建立的凝胶渗透色谱-液相色谱法准确可靠,能应用于沉积物中多环芳烃的测定;优化仪器条件,规范实验操作提高回收率能减小方法不确定度。     

Early prenatal exposure to MPTP does not affect nigrostrial neurons in macaque monkey

The discovery of 1‐methyl‐4‐phenyl‐1,2,3,6‐tetrahydropyridine (MPTP), a toxin that induces parkinsonism in both human and primate, has prompted the search for environmental toxins potentially responsible for idiopathic Parkinson's disease (PD). The present study reports the ultimate effects of MPTP intoxication of a female macaque monkey, which unraveled to be pregnant after parkinsonism had developed, upon its fetus. Detailed examination of the offpsring nigrostriatal pathway showed that tyrosine hydroxylase immunoreactivity in caudate‐putamen nuclei and substantia nigra compacta (SNc) was not different from an age‐matched control. Biochemical analysis of the tissue content of dopaminergic markers further suggested modification of metabolism in the MPTP‐exposed monkey. These data suggest that early prenatal intoxication does not destroy nigrostriatal neurons, most likely because dopamine neurons had not developed yet when exposed to MPTP. Synapse 70:52–56, 2016. © 2015 Wiley Periodicals, Inc.     

气相色谱法测定苦豆子提取物中乙醇残留量

目的：建立苦豆子提取物中乙醇残留量的气相色谱测定方法。方法：采用高效气相色谱法测定乙醇残留量,Agilent HP－IN－NOWAX毛细管柱为样品分析柱,甲醇为稀释剂,FID检测器温度220℃,进样口温度190℃,分流比为20∶1,外标法测定乙醇残留量。结果：测定的乙醇浓度与峰面积的相关系数为0.99944,回收率在96.0%～99.7%之间,重复性RSD为1.24%。结论：本方法可用于苦豆子提取物中乙醇残留量的测定。     

毛细管气相色谱法测定多西他赛注射液溶剂中乙醇含量的方法学验证

目的：建立多西他赛注射液溶剂中乙醇含量的气相色谱测定方法。方法：气相色谱法：毛细管色谱柱;载气：氮气;检测器：氢火焰离子化检测器;起始温度为50℃,维持10min,再以每分钟10℃的速率升温至110℃;进样口温度：190℃;检测器温度：220℃;柱流量：3.2ml/min;进样量：1μl。结果：定量限、检测限、溶液稳定性、线性、耐用性、重复性、进样精密度经验证,结果均良好。结论：本法可用于多西他赛注射液溶剂中乙醇含量的测定。     

注射用头孢曲松钠他唑巴坦钠(3:1)含量测定方法的研究

目的 建立同时测定注射用头孢曲松钠他唑巴坦钠中头孢曲松和他唑巴坦含量的方法。 方法 色谱柱为DIKMA Diamonsil C18柱(4.6 mm×250 mm, 5 µm);流动相A为0.03 mol/L磷酸二氢钾溶液-10%四丁基氢化铵溶液(995:5),用磷酸调pH至3.0,流动相B为乙腈：甲醇(1:2),以A:B=70：30作为流动相;波长为230 nm;流速为1.0 ml/min;柱温为30℃。结果 头孢曲松和他唑巴坦之间的分离度为2.89,头孢曲松和反式头孢曲松的分离度为12.41;酸、碱、氧化、高温和光照破坏试验表明,头孢曲松和他唑巴坦与其它杂质的分离度良好。头孢曲松和他唑巴坦的进样量在线性范围内进样量和峰面积呈良好的线性关系,相关系数分别为1和0.9999;平均加样回收率分别为100.3%和99.5%,RSD分别为0.90%和0.66%。结论 该方法操作简便,专属性和耐用性好,结果准确,可同时测定注射用头孢曲松钠他唑巴坦钠中头孢曲松和他唑巴坦的含量。     

RP-HPLC法同时测定人血清中4种抗癫痫药的浓度

目的：建立同时测定人血清中拉莫三嗪(LTG)、苯巴比妥(PB)、苯妥英(PHT)和卡马西平(CBZ)浓度的高效液相色谱法。方法血清样品经甲醇沉淀蛋白后直接进样测定。色谱柱采用Waters Symmetry C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-水(55∶45),检测波长235 nm。结果 LTG、PB、PHT和CBZ的线性范围分别是1.56~50、3.13~100、2.19~70、1.09~35μg/ml,平均回收率均>98%。结论本方法操作简便,结果准确,适用于临床治疗药物监测。     

Riboflavin concentration in corneal stroma after intracameral injection

AIM:To evaluate the enrichment of riboflavin in the corneal stroma after intracameral injection to research the barrier ability of the corneal endothelium to riboflavin in vivo.METHODS:The right eyes of 30 New Zealand white rabbits were divided into three groups. Different concentrations riboflavin-balanced salt solutions (BSS) were injected into the anterior chamber (10 with 0.5%, 10 with 1%, and 10 with 2%). Eight corneal buttons of 8.5 mm in diameter from each group were dissected at 30min after injection and the riboflavin concentrations in the corneal stroma were determined using high-performance liquid chromatography (HPLC) after removing the epithelium and endothelium. The other two rabbits in every group were observed for 24h and sacrificed. As a comparison, the riboflavin concentrations from 16 corneal stromal samples were determined using HPLC after instillation of 0.1% riboflavin-BSS solution for 30min on the corneal surface (8 without epithelium and 8 with intact epithelium).RESULTS: The mean riboflavin concentrations were 11.19, 18.97, 25.08, 20.18, and 1.13 μg/g for 0.5%, 1%, 2%, de-epithelialzed samples, and the transepithelial groups, respectively. The color change of the corneal stroma and the HPLC results showed that enrichment with riboflavin similar to classical de-epithelialized corneal collagen crosslinking (CXL) could be achieved by intracameral1% riboflavin-BSS solution after 30min; the effect appeared to be continuous for at least 30min.CONCLUSION:Riboflavin can effectively penetrate the corneal stroma through the endothelium after an intracameral injection in vivo, so it could be an enhancing method that could improve the corneal riboflavin concentration in transepithelial CXL.     

Application of HPLC mixed‐mode chromatography in determining radiochemical purity of [14C] labeled metformin hydrochloride

Metformin is currently prescribed worldwide to treat type 2 diabetes, and therefore, radiolabeled [¹⁴C] metformin is often prepared for clinical comparisons of new drug candidates. Prior to using the radiolabeled metformin, the purity needs to be determined to ensure the quality of the material. While typical reversed‐phase LC methods are often the first choice for purity analysis, they are not suitable for this determination because the compound is poorly retained under these conditions. Mixed‐mode chromatography has been demonstrated to overcome these retention issues, and therefore, this methodology was utilized for the purity determination of radiolabeled metformin.     

薄荷水质量控制方法的研究

目的 完善薄荷水的质量控制方法。方法 采用薄层色谱法鉴别薄荷水中的薄荷素油,用气相色谱法测定薄荷水中薄荷脑的含量。结果 薄层色谱法鉴别专属性强;气相色谱法中,薄荷脑线性范围为5.0~80.0μg/ml(r=0.999 9),平均回收率为103.16%,RSD为1.81%。结论 该法操作简便,结果准确,灵敏度高,重复性好,可有效地控制薄荷水的质量。