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正常人尿中草酸盐含量低,已有的测定方法均不够精确、灵敏,或过于繁琐费时。本文介绍一种精确、简便而快速测定尿中草酸盐的气相色谱法。原理用氯化钙沉淀尿中草酸盐,再将其转变为二甲基草酸酯后,用气相色谱仪测定。方法用塑料瓶收集并量出24小时尿量,取200毫升尿样酸化至pH1.0,置50～55℃水浴30分钟,以溶解其原有的草酸钙结晶,滤纸过滤。取上述已酸化的尿液40毫升置50毫升的圆底离心管中,加入含200毫微克(5.6×10~4cpm)~(14)C-草酸(98%放化纯)的溶液100微升和2毫克草酸,用4M氢氧化铵调溶液至pH8.0(用pH计),再用6M醋酸调至pH5.2(操作过程中连续用磁力搅拌)。加氯化钙溶液(100克/升)1毫升,使草酸钙沉淀,并置室温下过夜。1000
Normal urine oxalate content is low, the existing determination methods are not precise enough, sensitive, or too complicated time-consuming. This article describes a precise, simple and rapid determination of urinary oxalate gas chromatography. Principle Calcium hydroxide precipitated urine oxalate, and then converted to dimethyl oxalate, determined by gas chromatography. Methods Collected and measured 24 hours urine volume with plastic bottle, take 200 ml of urine sample acidified to pH1.0, set 50 ~ 55 ℃ water bath for 30 minutes to dissolve its original calcium oxalate crystals, filter paper filtration. Take 40 ml of the acidified urine into a 50 ml round bottom centrifuge tube and add 100 μl of a solution containing 200 ng (5.6 × 10 ~ 4 cpm) ~ (14) C-oxalic acid (98% radiochemical purity) And 2 mg of oxalic acid. The solution was adjusted to pH 8.0 (pH value) with 4 M ammonium hydroxide and adjusted to pH 5.2 with 6 M acetic acid (continuous magnetic stirrer during operation). Add 1 ml of calcium chloride solution (100 g / L) to precipitate calcium oxalate and allow to stand overnight at room temperature. 1000