液相色谱-串联质谱法(LC-MS/MS)测定氢氯噻嗪中三种氯苯胺含量  

Determination of three chloroanilines in hydrochlorothiazide by liquid chromatography-tandem mass spectrometry(LC-MS/MS)

作　　者：黄茹婷 马卫兴 董淑波 HUANG Ru-ting;MA Wei-xing;DONG Shu-bo(College of Pharmacy,Jiangsu Ocean University,Lianyungang 222005,China;Jiangsu Deyuan Pharmaceutical Co.,LTD.,Lianyungang 222000,China;School of Biomedical Industry,Jiangsu Ocean University,Lianyungang 222005,China)

机构地区：[1]江苏海洋大学药学院,江苏连云港222005 [2]江苏德源药业股份有限公司,江苏连云港222000 [3]江苏海洋大学生物医药产业学院,江苏连云港222005

出　　处：《化学研究与应用》2024年第2期372-379,共8页Chemical Research and Application

摘　　要：建立液相色谱-串联质谱法(LC-MS/MS)测定氢氯噻嗪中三种氯苯胺的含量,色谱柱选用(CHIRALCEL??OJ-RH,150 mm×4.6 mm,5μm),离子源采用大气压化学电离源(APCI),使用正离子扫描模式;检测模式为选择反应监测(SRM)。结果显示,邻氯苯胺、间氯苯胺和对氯苯胺分别在0.76 ng·mL^(-1)~30.55 ng·mL^(-1)、0.76 ng·mL^(-1)~30.26 ng·mL^(-1)和0.76 ng·mL^(-1)~30.44 ng·mL^(-1)范围内线性良好,定量限均为0.76 ng·mL^(-1),检测限均为0.25 ng·mL^(-1);平均加标回收率分别为94.02%、93.27%和90.09%,RSD分别为2.69%、3.84%、3.19%,且稳定性良好。样品检测结果显示6批均未检出三种杂质,建立的分析方法重复性好、专属性强、灵敏度高,适用于氢氯噻嗪中三种氯苯胺的检测。Objective To establish a liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for the determination of three chloroanilines in hydrochlorothiazide.The chromatographic column was CHIRALCEL OJ-RH,150 mm×4.6 mm,5μm,the ion source was APCI,and the positive ion scanning mode was used.The detection mode was selective response monitoring(SRM).The results showed that o-chloroaniline,m-chloroaniline and p-chloroaniline had good linearity in the range of 0.76 ng·mL^(-1)~30.55 ng·mL^(-1),0.76 ng·mL^(-1)~30.26 ng·mL^(-1),0.76 ng·mL^(-1)~30.44 ng·mL^(-1),and the limits of quantitation were all 0.76 ng·mL^(-1).The detection limit were 0.25 ng·mL^(-1).The average recoveries were 94.02%,93.27%and 90.09%,RSDS were 2.69%,3.84%and 3.19%,respectively,with good stability.The results of sample detection showed that no three impurities were detected in the 6 batches.The established analytical method has good repeatability,strong specificity and high sensitivity,and is suitable for the detection of three chloroanilines in hydrochlorothiazide.

关 键 词：LC-MS/MS 氢氯噻嗪 邻氯苯胺 间氯苯胺 对氯苯胺 

分 类 号：O657[理学—分析化学]