液相色谱-离子阱质谱法同时检测食品和药品中非法添加的17种激素  

Simultaneous Detection of 17 Kinds of Glucocorticoids Illegally Added in Food and Medicine by Liquid Chromatography-Ion Trap Mass Spectrometry

作　　者：刘静 董宇 王震红 LIU Jing;DONG Yu;WANG Zhen-hong(Liaoning Inspection,Examination&Certification Centre,Shenyang 110036,China;Liaoning Institute for Drug Control,Shenyang 110036,China)

机构地区：[1]辽宁省检验检测认证中心,辽宁沈阳110036 [2]辽宁省药品检验检测院,辽宁沈阳110036

出　　处：《食品与药品》2025年第1期31-37,共7页Food and Drug

基　　金：辽宁省市场监督管理局科技计划项目(编号:2022ZC006);辽宁省科技厅科技计划项目(编号:2023-MSLH-088)。

摘　　要：目的建立液相色谱-离子阱质谱法(LC-ITMS)同时检测食品和药品中非法添加的17种糖皮质激素的分析方法。方法不同基质类型(片剂、颗粒剂、胶囊剂、茶剂、散剂、口服液、乳膏剂、软膏剂、丸剂、搽剂、洗剂等)的样品经乙腈提取后,采用大曹三耀CAPCELL-PAK ADME(4.6 mm×150 mm,3μm)色谱柱进行分离,采用乙腈-0.02 mol/L乙酸铵溶液(含0.2%冰乙酸)为流动相,以梯度洗脱方式进行分析。利用正离子电喷雾离子源(ESI﹢)对非法添加的17种糖皮质激素类化合物进行检测。通过比较样品溶液和对照溶液的色谱图及质谱图信息,定性分析样品中糖皮质激素的非法添加情况。结果17种化合物的色谱峰分离度均符合要求,方法的最低检出限为0.8~10.0 ng/ml。37批样品中共计8批样品检出醋酸泼尼松,2批样品检出地塞米松,1批样品检出丙酸氯倍他索,1批样品检出倍他米松,被测样本中糖皮质激素的阳性检出率为32%。结论该检测方法简单、快速、特异性强,准确可靠,可用于食品和药品中非法添加的17种糖皮质激素类化学成分的快速检测。Objective To establish a high performance liquid chromatography-ion trap mass spectrometry(HPLC-ITMS)method for the simultaneous determination of 17 glucocorticoids illegally added in medicine and food.Methods Samples of different matrix types(tablets,granules,capsules,medicinal tea,powder,oral liquid,cream,ointment,pills,liniment,lotion)were extracted by acetonitrile and separated on a CAPCELLPAK ADME column(4.6 mm×150 mm,3μm),using acetonitrile and 0.02 mol/L ammonium acetate solution(containing 0.2%of glacial acetic acid)as the mobile phase of gradient elution.The electrospray ionization source in positive ion scanning mode(ESI﹢)was used to detect 17 glucocorticoid compounds illegally added.The qualitative analysis of 17 glucocorticoids was performed by comparing the chromatograms and mass spectrograms of the test solution and the reference solution.Results The 17 compounds were completely separated under the selected LC-ITMS condition.The detection limits were all in the range of 0.8-10.0 ng/ml.A total of 37 batches of commercial samples were analyzed and prednisone acetate was detected in 8 batches of samples,dexamethasone was detected in 2 batches of samples,clobetasol propionate was detected in 1 batch of sample and betamethasone was detected in 1 batch of sample.The positive detection rate of glucocorticoids in the tested samples was 32%.Conclusion This method is easy to operate,specific and reliable,and is suitable for the rapid determination of illegal addition of 17 glucocorticoids in drug and food.

关 键 词：液相色谱-离子阱质谱联用法 糖皮质激素 非法添加 

分 类 号：R927[医药卫生—药学]