高效液相色谱-串联质谱法同时测定盐酸拉贝洛尔中三种杂质
郝丽娟，苗会娟，韩佳芮，徐欢欢，王茉莉，徐艳梅
1. 河北省药品医疗器械检验研究院，国家药品监督管理局仿制药质量控制与评价重点实验室，石家庄 050227； 2. 河北科技大学，石家庄 050091
Simultaneous determination of three impurities in Labetalol Hydrochloride by high performance liquid chromatography-tandem mass spectrometry
, HAO Lijuan1, MIAO Huijuan1, HAN Jiarui2, XU Huanhuan1 WANG Moli1, XU Yanmei1
1. Hebei Institute for Drug and Medical Device Control, NMPA Key Laboraory for Quality Control and Evaluation of Generic Drug,Shijiazhuang 050227, China; 2. Hebei University of Science and Technology, Shijiazhuang 050091, China
摘要：建立高效液相色谱-串联质谱法同时测定盐酸拉贝洛尔中 2-羟基-5-［1-羟基 -2-［（1-甲基 -3-苯丙基）氨基］乙基］苯甲酸、2-羟基-5-［1-羟基-2［（-1-甲基-3-苯丙基）氨基］乙基］苯甲酸甲酯和 2-羟基-5-（2-（4-苯基丁-2-氨基）乙酰）苯甲酰胺的含量。 采用 Agilent Eclipse XDB-C18柱（250 mm×4.6 mm，5 μm）为分离柱，以 0.1%（质量分数）的乙酸溶液为流动相 A，乙腈-0.1% 的乙酸溶液（体积比为 1∶1）为流动相 B，流量为 1.5 mL/min，梯度洗脱，柱温为 40 ℃，进样体积为 10 μL，离子源为大气压化学电离源，采用多反应监测模式。三种杂质的质量浓度分别在 1.0160～203.20、1.0320～206.40、1.0370～207.40 ng/mL 范围内与色谱峰面积线性相关，相关系数均大于 0.999，3 种化合物的检出限均为 0.03 ng/mL，定量限均为 0.10 ng/mL。 样品平均回收率分别为 95.3% 、92.4%、91.9%，测定结果的相对标准偏差分别为1.44%、1.46%、1.11%（n=9）。该方法可用于同时测定盐酸拉贝洛尔中 3 种杂质，有效地监测盐酸拉贝洛尔的质量。
Abstract：A method was established for the simultaneous determination of 2-hydroxy-5- [1-hydroxy-2- [(1-methyl-3- phenylpropyl) amino] ethyl] benzoic acid, 2-hydroxy-5- [1-hydroxy-2- [(1-methyl-3-phenylpropyl) amino] ethyl]benzoic acid methyl ester and 2-hydroxy-5- (2- (4-butyl phenyl-2-amino) acetyl) benzamide in Labetalol Hydrochloride by high performance liquid chromatography-tandem mass spectrometry. Agilent Eclipse XDB-C18 column (250 mm ×4.6 mm, 5 μm) was used as the separation column, 0.1% (mass fraction) acetic acid solution was used as mobile phase A, acetonitrile- 0.1% acetic acid solution (volume ratio was 1: 1) was used as mobile phase B, gradient elutionat with the flow rate of 1.5 mL/min, the column temperature was 40 ℃, and injection volume was 10 μ L. The ion source was atmospheric pressure chemical ionization source, and the multiple reaction monitoring mode was adopted. The mass concentrations of the three impurities had a good linear relationships with the chromatographic peak area in the range of 1.0160-203.20, 1.0320- 206.40, 1.0370-207.40 ng/mL, respectively, the correlation coefficients were all more than 0.999. The detection limits of the three compounds were all 0.03 ng/mL, and the quantification limits were all 0.10 ng/mL. The average recovery rates of the samples were 95.3%, 92.4% and 91.9%, respectively. The relative standard deviations of the determination results were 1.44%, 1.46% and 1.11%, respectively (n=9). The method can be used for the simultaneous determination of three impurities in Labetalol Hydrochloride, and the quality of labetalol hydrochloride can be monitored.
关键词：高效液相色谱-串联质谱法；盐酸拉贝洛尔；2-羟基-5-［1-羟基-2-［（1-甲基-3-苯丙基）氨基］乙基］苯甲酸；2-羟基-5-［1-羟基-2［（-1-甲基-3-苯丙基）氨基］乙基］苯甲酸甲酯；2-羟基-5-（2-（4-苯基丁-2-氨基）乙酰）苯甲酰胺
Keywords：high performance liquid chromatography-tandem mass spectrometry; Labetalol Hydrochloride; 2-hydroxy-5-[1-hydroxy-2-[(1-methyl-3-phenylpropyl)amino]ethyl]benzoic acid; 2-hydroxy-5-[1-hydroxy-2-[(1-methyl-3-
基金：河北省卫生健康委科研基金项目（20211193）
本文引用格式：
郝丽娟，苗会娟，韩佳芮，等.高效液相色谱-串联质谱法同时测定盐酸拉贝洛尔中三种杂质[J].化学分析计量，2023，32(10)：11.
HAO Lijuan，MIAO Huijuan，HAN Jianrui，et al. Simultaneous determination of three impurities in Labetalol Hydrochloride by highperformance liquid chromatography-tandem mass spectrometry[J]. Chemical Analysis and Meterage，2023，32(10)：11.
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