气相色谱法测定乌洛托品含量的研究

使用邻苯二甲酸二甲酯作为内标,建立毛细管气相色谱法测定原料药中乌洛托品的含量。色谱柱为HP-5石英毛细管柱(30m×0.32mm×0.25μm),FID检测器,内标法定量。结果表明:在确定的色谱条件下,乌洛托品浓度在8.42~538.80μg/mL范围内,线性关系良好,线性回归方程A=0.177 0c+0.353 7(c:μg/mL),r2=0.999 7;加标回收率在96.83%~101.24%之间,相对标准偏差度为3.84%(n=6),最低检出限为1.54ng,最低定量限为4.98ng。该方法灵敏度和准确度均符合要求,方法可靠,可用于乌洛托品含量的测定。

Study on the determination of methenamine by gas chromatography

A capillary gas chromatography （CGC） method using dimethyl phthalate as the internal standard was established for the determination of methenamine in pharmaceutical product.HP-5 silici -capillary column （30 m × 0.32 mm × 0.25 μm） was adopted for the determination.FID detector and internal standard method were used for the quantitative analysis.The linear relation of formaldehyde was all right with the concentration in the range of 8.42 ～ 538.80 μg/mL under the definite chromatographic condition.The linear regression equation was A =0.177 0c ＋0.353 7 （c：μg/mL）,r2 =0.999 7.The addition standard recoveries were ranging from 96.83％ to 101.24％ and RSD was 3.84％ （n =6）.The detection limit was 1.54 ng.The limit of quantization was 4.98 ng.Both the sensitivity and accuracy fitted the bill.This method can be successfully used in the determination of methenamine in urotropine raw material.