顶空气相色谱法检测原料药氯沙坦钾中的残留溶剂.PDFVIP

顶空气相色谱法检测原料药氯沙坦钾中的残留溶剂  陈盼盼 1 ，刘璇 1 ，王丹华 2 ，王宏亮 1(1.临海市食品药品检验检测中心，浙江 台州 317000 ；2. 台州职业技术学院，浙江 台州 318000) 摘要：目的 建立顶空气相色谱法测定氯沙坦钾原料药有机残留溶剂的方法。方法 选用 Agilent 7890 气相色谱仪，配 备 7697 顶空进样器，DB-624 毛细管色谱柱作为分析柱，FID 检测器，外标法测定；并对分析方法建立进行研究。结果 甲 醇、异丙醇、乙酸乙酯、环己烷、甲苯分别在 0.122~90.2 ，0.28~151.3 ，0.03~61.4 ，0.22~76.4 ，0.035~26.8 μg·mL1 线性 关系良好(r0.999) ；各组分检测限分别为 0.037 ，0.090 ，0.009 ，0.070 ，0.012 μg·mL1 ；各组分平均回收率为 90.0%~110.0% 。 结论 该方法简单、可靠、准确，可用于原料药氯沙坦钾有机残留溶剂的测定。 关键字：气相色谱法；顶空；原料药；氯沙坦钾；残留溶剂 中图分类号：R917 文献标识码：B 文章编号：1007-7693(2017)07-1015-03 DOI: 10.13748/ki.issn1007-7693.2017.07.018 引用本文：陈盼盼, 刘璇, 王丹华, 等. 顶空气相色谱法检测原料药氯沙坦钾中的残留溶剂[J]. 中国现代应用药学, 2017, 34(7): 1015-1017. Determination of Residual Solvents in Losartan Potassium by Head Space Gas Chromatography 1 1 2 1 CHEN Panpan , LIU Xuan , WANG Danhua , WANG Hongliang (1.The Inspection Testing Center of Food and Drug in Linhai, Taizhou 317000, China; 2.Taizhou Vocational Technical College, Taizhou 318000, China) ABSTRACT: OBJECTIVE To establish a head space gas chromatography method for determination of residual solvents in active pharmaceutical ingredients of losartan potassium. METHODS Agilent 7890 gas chromatography with 7697 head space sampling and FID detector was selected. And DB-624 capillary column was used as analytical column. External standard method was used to determine the content. The analytical method was also explored. RESULTS A good linear correlation of methanol, isopropanol, ethyl acetate, cyclohexane and toluene were showed at the range of 0.12290.2, 0.28151.3, 0.0361.4, 0.2276.4 and 0.03526.8 μg·mL1 with r0.999, respectively. Detection limit of each components was 0.037, 0.090, 0.009, 0.070, 0.012 μg·mL1, respectively; Recovery range