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LC-MS测定罗库溴铵缩合物中环氧物的含量
引用本文:吴水仙, 王咏, 龚伟青. LC-MS测定罗库溴铵缩合物中环氧物的含量[J]. 中国现代应用药学, 2012, 29(6): 539-541.
作者姓名:吴水仙  王咏  龚伟青
作者单位:1.浙江仙琚制药股份有限公司,浙江 台州 317300
摘    要:
目的 采用液相色谱-四级杆质谱法(LC-MS)建立罗库溴铵缩合物中环氧物的检测方法。 方法 色谱柱为Agilent Eclipes XDB-C18(150 mm×2.1 mm,3 μm),以甲醇-0.1%甲酸溶液为流动相进行梯度洗脱,流速:0.25 mL min-1,柱温:30 ℃,SIM离子采集方式,采集离子分子量:347.2,APCI离子源,进样量:5 μL。结果 环氧物的定量限为0.000 3%,检测限为0.000 09%,柱温、流速的微小变化不影响检测结果,定量限浓度平均回收率为98.9%(n=3)。结论 本方法灵敏高,准确度高,可用于罗库溴铵缩合物中环氧物限量检测。

关 键 词:罗库溴铵  环氧物  液质联用  检测
收稿时间:2011-05-27
修稿时间:2012-03-06

Determination of Epoxy Compound in Rocuronium Bromide Condensation Compound by LC-MS
WU Shuixian, WANG Yong, GONG Weiqin. Determination of Epoxy Compound in Rocuronium Bromide Condensation Compound by LC-MS[J]. Chinese Journal of Modern Applied Pharmacy, 2012, 29(6): 539-541.
Authors:WU Shuixian  WANG Yong  GONG Weiqin
Affiliation:1.Zhejiang Xianju Pharmaceutical Co. Ltd., Taizhou 317300, China
Abstract:
OBJECTIVE To establish a LC-MS method for the determination of epoxy compound in rocuronium bromide condensation compound. METHODS The analysis was carried out on an Agilent Eclipes XDB-CI8 column(150 mm×2.1 mm, 3μm), using a gradient elution of methanol and 0.1% formic acid as the mobile phase at a flow rate of 0.25 mL-min-1 at 30 ℃, ion source was APCI, acquisition mode was SIM positive ionization, and selected ion was m/z 347.2 ([M+H]+). RESULTS The LOQ was 0.000 3%, the LOD was 0.000 09%; there was no influence on sample testing when small changes were made in the chromatographic conditions; the average recovery was 98.9% with RSD of 8.41%(n=3). CONCLUSION The method was sensitive, accurate, and suitable for the limit determination of epoxy compound in rocuronium bromide condensation compound.
Keywords:Rocuronium Bromide   Epoxy Compound   LC-MS   Determination
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