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目的 建立氢溴酸替格列汀中遗传毒性杂质溴乙烷残留量的气相色谱(GC)检测方法。方法 采用迪马DM-624色谱柱(30 m×0.53 mm×3.0 μm);电子捕获检测器(ECD);程序升温:初始柱温40 ℃,保持3 min,以20 ℃/min升温至200 ℃,保持5 min;进样口温度:210 ℃;检测器温度:210 ℃;载气:氮气;分流比:3:1;进样量1 μL。结果 溴乙烷在0.75~6.75 μg/mL与峰面积呈良好的线性关系(r=0.999 7),最低检测限为0.26 μg/mL。平均回收率为99.4%,RSD值为0.3%(n=9)。3批氢溴酸替格列汀样品中均未检测出溴乙烷。结论 该方法简便、准确,重复性好,适用于氢溴酸替格列汀中溴乙烷残留量的控制。 相似文献
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Catherine A. Picut Hiroaki Aoyama James W. Holder Lois Swirsky Gold Robert R. Maronpot Darlene Dixon 《Experimental and toxicologic pathology》2003,55(1):1-9
Chloroethane, bromoethane and ethylene oxide represent a unique set of chemicals that induce endometrial neoplasms in the uterus of B6C3F1 mice following an inhalation route of exposure. The results of the NTP's chronic bioassays with these three compounds resulted in an unusually high incidence of uterine epithelial neoplasms in B6C3F1 mice (chloroethane 86%, bromoethane 56%) and a lower incidence for ethylene oxide (10%). The uterine neoplasms were classified as adenomas, adenocarcinomas, and squamous cell carcinomas for bromoethane, and as adenocarcinomas for both chloroethane and ethylene oxide. The adenocarcinomas and squamous cell carcinomas were invasive into the myometrium and the serosa, and metastasized to a wide variety of organs. Metastatic sites included most commonly the lung, lymph nodes, and ovary at unusually high rates of metastases (79% for chloroethane and 38% for bromoethane). Because of the dramatically high rates of uterine neoplasms (induced by chemicals given by the inhalation route) and metastases, a re-evaluation of the pathology and incidence data was undertaken. The earlier results were confirmed. The mechanism of uterine carcinogenesis by chloroethane, bromoethane and ethylene oxide is unclear. 相似文献
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目的:建立氢溴酸替格列汀中遗传毒性杂质溴乙烷残留量的气相色谱(GC)检测方法。方法采用迪马 DM-624色谱柱(30 m×0.53 mm×3.0μm);电子捕获检测器(ECD);程序升温:初始柱温40℃,保持3 min,以20℃/min升温至200℃,保持5 min;进样口温度:210℃;检测器温度:210℃;载气:氮气;分流比:3∶1;进样量1μL。结果溴乙烷在0.75~6.75μg/mL与峰面积呈良好的线性关系(r=0.9997),最低检测限为0.26μg/mL。平均回收率为99.4%,RSD值为0.3%(n=9)。3批氢溴酸替格列汀样品中均未检测出溴乙烷。结论该方法简便、准确,重复性好,适用于氢溴酸替格列汀中溴乙烷残留量的控制。 相似文献
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