2014-阿格列汀测定相关22.docxVIP

查阅文献应该记录的内容:阿格列汀（吡格列酮苯酸酯），分子量461.51。溶于二甲基亚砜，微溶于水和甲醇及乙醇，溶于乙腈?极微溶于辛醇和乙酸异丙酯。PKa=9.47；极性35.44。用0.01 mol/LHCl溶解，47.0, 27.1, 27.6 and 21.9 mg/ml溶解于 0.1mol/LHCl(pH 1.0),,0.01mol/LHCl(pH 2.0),（实验显示溶解度与pH无关）pH 4.5 ，0.05mol醋酸缓冲液和 pH 6.8,0.05mol磷酸缓冲液, 一种二肽基肽酶-4（DPP-4）抑制剂药动学参数 800mg TMAX1-2小时，消除半衰期21小时（剂量为25mg）,分布容积417L.代谢:两个主要代谢产物M-1和M-2，1为活性代谢产物，但小于母体的1%,2为非活性代谢产物，不转换为S构型，25mg剂量检测不到S-构型。肾排泄率9.6?L/hr50mg剂量线性范围1.07 to 347 ng/mL。来源离子对/类型质谱参数（参考）液相条件萃取方法线性范围；给药剂量；峰浓度溶剂备注Effects of DPP-4 Inhibitors on the Heart in a Rat Model of Uremic CardiomyopathyFocus 96-well extraction plates，固相萃取Rats,定量下线0.250 nmol/l，C13作内标，Pharmacokinetics,Pharmacodynamics, and Tolerability of Single Increasing Doses of the Dipeptidyl Peptidase–4 Inhibitor Alogliptin in Healthy Male SubjectsRonald Christopher, PhD1，March 2008PositiveMRM 340/116, 326/116, 382 / 126梯度洗脱，水相（0.1%甲酸）/有机相乙腈（0.1%甲酸）a 3-mm internal diameter (ID) × 4 mm guard column. a 2-mm ID × 50 mm analytic columna binary HPLC pump乙腈蛋白沉淀法alogliptin 25, 50, 100, 200, 400, or 800 mg160μL 水：甲醇(80:20 )氘化内标25/100微升，保留时间（阿格列汀/M-1/M-2=~2.4/~1.9/~2.3 minutes）还测定了S-阿格列汀,以及尿液中的各物质浓度，及血液中二肽基肽酶-4酶的分析活性胰高血糖素样肽-1测定Pharmacokinetic, Pharmacodynamic, and Tolerability Profiles of the Dipeptidyl Peptidase–4 Inhibitor Alogliptin: ARandomized, Double-Blind, Placebo-Controlled, Multiple-Dose Study in Adult Patients with Type 2 DiabetesPaul Covington, MD1，March 2008质谱条件同上测定了阿格列汀和N-去甲基化活性代谢产物M-I，阿格列汀（1.00 to 1000 ng/mL；M-1(0.100 to 100 ng/Ml；)；剂量25,100,400；146，630，2420乙二胺4醋酸（抗凝剂），收集了血液和尿液。文中包含取血时间点等信息。代谢物M-1为母体化合物的约1%，考虑为次代谢产物，没有测HPLC法测定苯甲酸阿格列汀片的含量时春娟1 2013年中国药房色谱柱：Kromasil C18（250 mm×4.6 mm，5 μm）；流动相：0.05 mol/L的KH2PO4溶液（磷酸调pH3.0）-乙腈（65 ∶35），流速：1.0 ml/min；检测波长：224 nm；柱温：室温；进样量：20 μl。19.96～179.6 μg/m流动相A NEW STABILITY INDICATING RP-HPLC METHOD DEVELOPMENT FOR SIMULTANEOUS ESTIMATION OF METFORMIN AND ALOGLIPTIN IN BULK AS WELL AS IN PHARMACEUTICAL FORMULATION BY USING PDA DETECTORG. Satya Sri*Indo American Journal of Pharmaceutical Research, 2013XTerra column (250 mm ×