超高效液相色谱-串联质谱法同时测定抗骨增生片中41种消炎止痛类化合物的含量  

Simultaneous Determination of 41 Anti-Inflammatory and Analgesic Compounds in Kangguzengsheng Tablets by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：黄晓姗 李沁 刘岩庭 陈海滨 陈在敏 HUANG Xiaoshan;LI Qin;LIU Yanting;CHEN Haibin;CHEN Zaimin(Fujian Institute for Food and Drug Quality Control,Fuzhou 350000,China)

机构地区：[1]福建省食品药品质量检验研究院,福州350000

出　　处：《理化检验（化学分册）》2024年第12期1246-1251,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：福建省药品监督管理局科技项目(2023008)。

摘　　要：取抗骨增生片样品20片,除去包衣后研细,取粉末1 g,加入50%(体积分数)甲醇溶液25 mL,在水温不超过60℃的条件下超声处理30 min,振摇混匀后过0.22μm滤膜,滤液采用超高效液相色谱-串联质谱法测定。在色谱分析中,以Welch Ultimate UHPLC XB-C18色谱柱(100 mm×2.1 mm,1.8μm)为固定相,不同体积比的乙腈-含5 mmol·L^(-1)乙酸铵的0.1%(体积分数)甲酸溶液的混合溶液为流动相进行梯度洗脱。在质谱分析中,以电喷雾离子源正、负离子模式电离,多反应监测模式检测,外标法定量。结果表明,41种消炎止痛类化合物的质量浓度在一定范围内和对应的定量离子峰面积呈线性关系,相关系数均大于0.9910,检出限(3S/N)为0.1~2μg·L^(-1);按照标准加入法进行回收试验,回收率为64.0%~114%,测定值的相对标准偏差(n=6)均小于11%。方法用于来自33个生产企业的57批样品的分析,均检出了阿司匹林,其来源值得进一步试验探究;3批样品检出了对乙酰氨基酚,推测来源于生产过程中的交叉污染。检出的阿司匹林和对乙酰氨基酚的含量均远低于对应药品的每日最小服用剂量。The 20 Kangguzengsheng tablet samples were taken,removed of the coating and ground finely.An aliquot(1 g)of powder was taken,and 25 mL of 50%(volume fraction)methanol solution was added.The mixture was ultrasonicated for 30 min at a water temperature not exceeding 60℃,shaken well and passed through a 0.22μm filter membrane.The filtrate was determined by ultra-high performance liquid chromatography-tandem mass spectrometry.In chromatographic analysis,a Welch Ultimate UHPLC XB-C18 column(100 mm×2.1 mm,1.8μm)was used as the stationary phase,and a mixture of acetonitrile and 0.1%(volume fraction)formic acid solution containing 5 mmol·L^(-1)ammonium acetate at different volume ratios was used as the mobile phase for gradient elution.In mass spectrometry,positive and negative ion modes of electrospray ion source were used for ionization,multiple reaction monitoring mode was used for detection,and external standard method was used for quantification.It was shown that linear relationships between the peak areas of the corresponding quantitative ions and mass concentrations of 41 anti-inflammatory and analgesic compounds were kept in definite ranges,with correlation coefficients greater than 0.9910 and detection limits(3S/N)of 0.1-2μg·L^(-1).Test for recovery was made according to the standard addition method,giving recoveries in the range of 64.0%-114%,and RSDs(n=6)of the determined values were less than 11%.The proposed method was used for the analysis of 57 batches of samples from 33 production enterprises,and aspirin was detected in all samples.The source of aspirin needed further experimental exploration.Acetaminophen was detected in 3 samples,presumable due to cross contamination during the production process.The detected levels of aspirin and acetaminophen were much lower than the minimum daily dose of the corresponding drugs.

关 键 词：抗骨增生片 超高效液相色谱-串联质谱法 非法添加 消炎止痛类化合物 

分 类 号：O657.63[理学—分析化学]