腐竹中乌洛托品的高效气相色谱检测技术

Detection technology on the methenamine in Yuba by gas chromatography

为了探讨研究腐竹等食品中乌洛托品的高效气相色谱检测方法,粉碎样品腐竹后,利用微波萃取仪以三氯甲烷为萃取剂充分萃取乌洛托品,然后浓缩移入离心管混匀离心,取其上清液进样.色谱条件:HP-5MS型毛细管柱30m×0.32mm,0.32μm;柱温条件为200℃;汽化室温度控制为200℃;进样方式:分流(分流体积比为30∶1),进样量为1.0μL;柱温程序:初始温度80℃,保持2min,以10℃/min的速率升温至185℃,保持10min;以体积分数99.995%的氮气为载气,流速控制为1.0mL/min.该种方法对乌洛托品的检出限为1mg/L,在线性范围内其线性相关系数为0.997 7.乌洛托品的回收率为104.02%,变异度为5.00%.该方法灵敏度高,选择性好,效能高,准确性好,所需试样少,应用范围广,快速方便,可以满足对腐竹中乌洛托品的分析要求.

In order to investigate the detection of methenamine in Yuba the methods of gas chromatog- raphy was set up. The method tried to crush Yuba. Then the methenamine in crushed Yuba was extracted in chloroform with microwave extraction instrument. Next, a centrifuge separated the supernatant and sample introduction. Chromatographic condition. HP-SMS capillary column 30 m× 0.32 mm, 0.32μm; Column temperature conditions of 200 ℃ ; vaporizer temperature control was 200 ℃ ; injection mode. split（split volume ratio 30：1）, injection volume 1.0μL; program of column temperature, initial start tem- perature of 80 ℃ for 2 rain, heated to 185 ℃ with 10 ℃/min, to maintain 10 mini volume fraction of 99. 995% nitrogen as the carrier gas flow rate was controlled for 1.0 mL/min. The limit of detection of the methenamine is 1 mg/L. The linear cor-relation coefficient is 0. 997 7 and recovery rate is 104.02%. The degree of variation is 5.00 %. The method has high sensitivity, high selectivity, high efficiency, good accu- racy, less the required sample, a wide range of applications quickly and easily to meet the requirements of the analysis of methenamine in Yuba.