采用GC和GC-MS法同时测定替卡西林钠及其制剂中的残留溶剂  

Simultaneous determination of residual organic solvents in ticarcillin disodium and its preparation by GC and GC-MS

作　　者：王茉莉 王强[1] 徐艳梅 张菁 张兰桐 Wang Mo-li;Wang Qiang;Xu Yan-mei;Zhang Jing;Zhang Lan-tong(The Drug Inspection Institute of Hebei Province,Shijiazhuang 050011;School of Pharmacy,Hebei Medical University,Shijiazhuang 050017)

机构地区：[1]河北省药品检验研究院,石家庄050011 [2]河北医科大学药学院,石家庄050017

出　　处：《中国抗生素杂志》2018年第10期1204-1210,共7页Chinese Journal of Antibiotics

摘　　要：建立顶空气相色谱法同时测定替卡西林钠及其制剂中的甲醇、乙醇、乙醚、丙酮、异丙醇、乙腈、乙酸乙酯等7种残留溶剂的含量,并采用气相色谱-质谱联用技术,结合质谱数据检索对样品中的其他挥发性杂质进行结构鉴定及含量测定。GC条件:色谱柱:DB-624毛细管柱(30m×0.25mm, 1.40μm);柱温:程序升温;检测器:氢火焰离子化检测器(FID);检测器温度:250℃;分流进样,分流比:10:1;进样口温度:200℃。GC-MS条件:色谱条件:除载气为氦气(He),流速为1.0mL/min外,其余条件同GC条件。质谱条件:离子源温度:230℃;传输线温度:250℃;接口温度:230℃;溶剂切割时间:4min;四极杆温度:150℃;采用电子轰击(EI)离子源;电离方式:电子能量70eV;扫描方式:全扫描(Full scan);扫描范围:m/z 30~500;检测时间:3.00~25.00min。7种残留溶剂之间的分离度良好,理论板数分别以其待测成分的色谱峰计算均不低于5000;甲醇、乙醇、乙醚、丙酮、异丙醇、乙腈、乙酸乙酯的线性范围分别为1.53~610.24、2.55~1020.76、2.55~1020.96、2.56~1014.96、2.53~1013.24、0.86~342.72和2.57~1026.76μg/m L(r2≥0.9983);平均回收率为89.2%~105.4%,RSD在2.2%~4.5%之间;检测限(LOD)≤0.86μg/m L;精密度的RSD≤2.3%;供试品溶液在12h内稳定性良好。该方法操作简便,准确度高,重现性好,在所考察的浓度范围内各组分线性关系良好,各色谱峰之间的分离度均符合要求。该方法为替卡西林钠及其制剂的质量控制提供了重要依据。To establish a method for the simultaneous determination of seven kinds of residual solvents in ticarcillin disodium and its preparation by headspace gas chromatography, such as methanol, ethanol, ether, acetone, isopropanol, acetonitrile and ethyl acetate. Using gas chromatography-mass spectrometry technology, the retrieval data for other volatile impurities in the sample were combined to identificate the structure and determinate the content. Headspace gas chromatography was adopted. The residual organic solvents were seperated on DB-624 （30m×0.25mm, 1.40μm） capillary column using temperature programming. The column temperature was maintained at 40℃ for 5min, and raised to 200℃ at a rate of 10℃/min, stayed for 4min. FID was used as detector with a temperature of 250℃. Split ratio： 10：1. The inlet temperature was 200℃. GC-MS conditions： chromatographic conditions： the carrier gas was helium （He） with the flow rate of 1.0mL/min, the remaining conditions accorded with GC conditions above. Mass spectrometry conditions： The interface temperature was set at 230℃. The transmission line temperature was 250℃.Ion source temperature： 230℃. Solvent cutting time： 4rain. Quadrupole temperature： 150℃. EI mode： 70eV. The mass spectrometer detector was in Full scan mode. Scan range： m/z 30-500amU. Detection time： 3.00-25.00min. The results showed that the separation of the seven kinds of residual solvents was good, and the theoretical plates were not less than 5000, respectively, with the chromatographic peaks of the components to be tested. The linear ranges of methanol, ethanol, ether, acetone, isopropanol, acetonitrile, ethyl acetate were 1.53-610.24μg/mL, 2.55-1020.76μg/mL, 2.55-1020.96μg/mL, 2.56-1014.96μg/mL, 2.53-1013.24μg/mL, 0.86-342.72μg/mL and 2.57-1026.76μg/mL （r^2≥0.9983）. The average recoveries were ranged from 89.2%-105.4% with the RSDs between 2.2% and 4.5%. LODs were not more than 0.86μg/mL, the RSD of precision were not more than 2.5%. The sample

关 键 词：替卡西林钠 顶空气相色谱法 有机溶剂 残留量 

分 类 号：R978.1[医药卫生—药品]