气相色谱-质谱法测定卡贝缩宫素注射液中12种亚硝胺

建立气相色谱-质谱法检测卡贝缩宫素注射液中12种亚硝胺的方法。以二氯甲烷作为萃取剂,萃取卡贝缩宫素注射液中的12种亚硝胺,萃取液经Thermo TG-WAX MS毛细管柱（30 m×0.25 mm,0.25μm）分离,采用气相色谱-质谱法检测,内标法定量。载气为高纯氦气,进样口温度为260℃,柱流量为1.0 mL/min,进样体积为2.0μL,柱温为40℃,传输线温度为230℃,离子源温度为280℃。12种亚硝胺的质量浓度在20～60 ng/mL范围内与色谱峰面积线性关系良好,相关系数均大于0.99,测定结果的相对标准偏差为0.49%～3.37%(n=6),平均回收率为79.39%～106.4%,检出限为1.000～3.003 ng/mL,定量限为3.000～10.01 ng/mL,溶液在室温放置24 h内稳定。该方法灵敏度高、准确度高、专属性强,可用于多肽类药物的亚硝胺检测。     

脂肪乳剂中微量维生素D2的分析

采用ALLTECH LiChrospher Si60色谱柱,以正己烷／异丙醇为流动相,通过叔丁基甲醚对维生素D2进行萃取,直接进行HPLC分离,对脂肪乳剂中维生素D2进行准确地测定。     

顶空-气相色谱法测定葡萄糖氯化钠注射液中12种溶剂残留量

建立顶空-气相色谱法测定葡萄糖氯化钠注射液中12种残留溶剂含量的方法。采用HP-INNOWAX毛细管色谱柱(60 m×320μm,0.5μm)为分离柱,检测器为氢火焰离子化检测器(FID),柱温为程序升温。12种残留溶剂乙醇、异丙醇、丙酮、丁酮、乙酸乙酯、乙酸丁酯、乙酸正丙酯、甲苯、乙苯、对二甲苯、邻二甲苯、间二甲苯均能完全分离,在考察的浓度范围内线性关系良好(r>0.995),检出限分别为0.055,0.019,0.023,0.070,0.155,0.013,0.003,0.009,0.004,0.004,0.004,0.005μg/mL。平均回收率为90.6%~109.0%,测定结果的相对标准偏差为2.2%~5.6%(n=9)。该方法专属性强,精密度、准确度和检测灵敏度高,重复性好,可用于葡萄糖氯化钠注射液中12种溶剂残留量的测定。     

反相高效液相色谱法测定己酮可可碱氯化钠注射液中己酮可可碱的含量

建立了反相高效液相色谱法测定己酮可可碱氯化钠注射液中己酮可可碱含量的方法。使用DiamansilC18柱 (15 0mm× 4 .6mmi.d .,5 μm) ,流动相为甲醇 -水 (体积比为 4 0∶6 0 ) ,流速为 1mL/min ,测定波长为 2 74nm。线性范围为 12 .5～ 30 0 .0 μg/mL ,线性回归方程为A =4 4 .6 6 2 8c - 17.119 2 ,相关系数r=0 .999 87,检出限为 5ng/mL。测量结果的相对标准偏差为 0 .5 4 % (n =6 ) ,平均回收率为 10 0 .81%。     

苦黄注射液中乙酸乙酯萃取物成分表征

用薄层分析、熔点测定、质谱、经外、核磁共振方法对苦黄注射液中酯溶性部分（乙酸乙要互可溶性部分）进行了成分分析,共鉴定了5种晶体,它们分别是大黄酚、大黄素甲醚、大黄酸、咖啡酸和没食子酸。     

反相高效液相色谱法测定甲强龙注射液中琥珀酸甲强龙和游离甲强龙 …

提出用十八烷基键合硅胶为填充剂的色谱柱，以乙腈－磷酸为流动相，同时测定甲强龙注射液中琥珀酸甲强龙和游离中强龙的含量，方法简便、准确、重现性好，两组分的分离效果好。     

流动注射化学发光抑制法测定抗坏血酸

基于抗坏血酸对Ｌｕｍｉｎｏｌ－ＫＩＯ４－Ｈ２Ｏ２体系化学发光反应的抑制作用,建立了化学发光抑制快速测定抗坏血酸的新方法。该方法线性范围为１．０＊１０＾－７－１．０＊１０＾－５ｍｏｌ／Ｌ,检出限为６．０＊１０＾－８ｍｏｌ／Ｌ,对８．０＊１０＾－７ｍｏｌ／Ｌ抗坏血酸１１次平行测定的相对标准偏差为１．０％。用于维生素Ｃ片剂及注射液中抗坏血酸含量的测定,结果令人满意。     

Electrochemical Study of Lincomycin on Au-PtNPs/nanoPAN/ Chitosan Nanocomposite Membrane and Its Determination in Injections

The Au-Pt alloy nanoparticles(Au-PtNPs) were electrochemically deposited on the surface of polyaniline nanotube(nanoPAN) and chitosan(CS) modified glassy carbon electrode(GCE). The electrochemical behavior of lincomycin at Au-PtNPs/nanoPAN/CS modified GCE was investigated by cyclic voltammetry, linear sweep voltammetry and chronocoulometry. Cyclic voltammetric experiments show that lincomycin at the nanocomposite membrane modified electrode exhibited a pair of quasi-reversible redox peaks in pH=6.0 PBS. The membrane could accelerate the electron transfer of lincomycin on the electrode and significantly enhance the peak current. In a range of 3.0―100.0 mg/L, the reductive peak current of lincomycin at 0.42 V was linearly related to its concentration and the linear regression equation was ip,c=0.2703ρ–0.0042(ip,c: μA; ρ: mg/L; r=0.998, n=7) with a detection limit of 1.0 mg/L(S/N =3). Compared with other methods, this method exhibited many advantages such as high sensitivity, selectivity, wide linear range and low detection limit. The method was used to determine the content of lincomycin in injections commercially available with satisfactory results. Some electrochemical parameters involved in the redox reaction of lincomycin, such as parameter of kinetic nα, standard rate constant ks and the number of H+, were also calculated.     

近红外光谱与组合的间隔偏最小二乘法测定清开灵四混液中总氮和栀子苷的含量

应用近红外光谱分析技术结合化学计量学方法, 建立了中药清开灵注射液中间体总氮和栀子苷含量测定的新方法. 首先采用Kernard-Stone法对训练集样本和预测集样品进行分类, 然后应用组合的间隔偏最小二乘法(Synergy interval partial least squares, siPLS)对所得近红外透射光谱进行有效谱段范围的选择以及二者定量校正模型的建立, 并对光谱预处理方法进行了详细的讨论. 所建立的总氮和栀子苷校正模型的预测相关系数(R)分别为0.999和0.708; 交叉验证误差均方根(RMSECV)均为0.023; 预测误差均方根(RMSEP)分别为0.074和0.159; 预测结果表明, 本实验所建方法快速、无损且可靠, 可推广并应用于中药注射液中间体的在线质量控制.