摘要
目前,主动性的现场稽查已成为市场监管的发展趋势,这需要在现场快速有效地筛查大量产品,评估是否含有非法添加化学药物,对有嫌疑的样品及时封存,再送至实验室进一步检验。离子迁移谱技术是近年来发展起来的快筛技术之一。实验采用固相萃取-离子迁移谱技术,建立了祛痘类化妆品中14种抗菌药物的快速筛查方法。对离子迁移谱检测条件、样品提取条件、固相萃取净化条件(固相萃取柱、淋洗液种类、洗脱液种类及体积)进行了详细考察与优化。最终使用80%(体积分数)乙腈水溶液(含0.2%(质量分数)三氯乙酸)作为样品提取溶液,提取后上样于活化后的弱阳离子交换柱(Oasis■ MCX固相萃取柱),3.0 mL甲醇淋洗,1.0 mL 2%氨水甲醇洗脱,洗脱液直接进离子迁移谱检测。14种抗菌药物的迁移时间在11~17 ms之间,检出限为0.2~1.2μg/g。同时,由于离子迁移谱法线性范围较窄,不能准确定量,建立了高效液色谱(HPLC)定量方法,用于固相萃取前处理步骤的优化和阳性样品的验证。25批化妆品样品中,筛查出1批阳性样品,与HPLC检测结果相符。该方法快速、简便、高效,显著降低了祛痘类化妆品基质对离子迁移谱检测14种抗菌药物的干扰,提高了检测灵敏度,有效降低了假阳性和假阴性的发生,可用于化妆品现场快速筛查,同时也扩大了离子迁移谱在化妆品等复杂基质中非法添加化学药物检测的应用范围。
The main methods currently used to detect illegally added chemicals in cosmetics include thin-layer chromatography,high performance liquid chromatography(HPLC),gas chromatography(GC),and liquid chromatography-mass spectrometry(LC-MS).Compared with other analytical techniques,these methods have the advantages of high sensitivity,specificity,and accuracy,all of which are required in practical detection work.However,they also present a number of limitations,such as long analysis times and requirements for skilled operators and strictly controlled laboratory environments.Supervision,a growing trend in market surveillance,requires rapid and effective methods to screen illegally added chemicals.The suspected samples are sealed for some time and then sent to the laboratory for further testing.Ion mobility spectrometry(IMS)is a new type of trace gas separation technology that was developed in recent years.The principle behind IMS is the separation and characterization of chemical species based on differences in the migration speed of their gas-phase ions under an electric field.As this technology has the advantages of miniaturization,easy operation,and quick responses,it is widely used in food and drug quality testing,as well as other related fields.However,it is rarely used in cosmetic detection,likely because the cosmetics matrix is highly complex,which can interfere with ion determination.Thus,optimizing the pretreatment process of cosmetics for IMS is important.In this work,solid-phase extraction(SPE)is combined with IMS to establish a method for the rapid screening of 14 antibacterial drugs in anti-acne cosmetics.The IMS detection parameters,sample extraction conditions,and SPE clean-up conditions(SPE column,type of leachate,type and volume of eluent)were studied and optimized in detail.The sample was extracted with 80%(v/v)acetonitrile aqueous solution(containing 0.2%(mass fraction)trichloroacetic acid),loaded onto an activated Oasis■ MCX SPE column,leached with 3.0 mL of methanol,and eluted with 1.0 mL of 2%ammonia methanol solution.The eluate was then directly injected into the IMS instrument.The IMS parameters were as follows:positive ion source voltage=2200 V,transfer tube voltage=8000 V,inlet temperature=180℃,transfer tube temperature=180℃,ion gate voltage=50 V,gate voltage pulse width=85μs,and migration gas flow rate=1.2 L/min.The migration times for the 14 antibacterial drugs ranged from 11 to 17 ms,and the detection limits for the target compounds ranged from 0.2 to 1.2μg/g.Owing to the narrow linear range of IMS,a quantitative method employing HPLC was also established to optimize the SPE pretreatment step and verify the positive samples.Chromatographic separation was conducted on a Phenomenex Luna C 18 column(250 mm×4.6 mm,5μm),with a column flow rate of 1.0 mL/min and gradient elution with mobile phases A(0.01 mol/L potassium dihydrogen phosphate adjusted to pH 4.0 with phosphoric acid)and B(acetonitrile).The column temperature was set to 35℃,and the injection volume was fixed at 5μL.A total of 25 cosmetics samples were screened,and one positive sample was found to be consistent with the results of HPLC.The proposed method is fast,simple,and efficient,and it can be used for the rapid screening of the 14 antibacterial drugs in anti-acne cosmetics.Pretreatment can significantly reduce the influence of the cosmetic matrices on the determination results,improve instrument sensitivity,and effectively decrease the occurrence rate of false positives and negatives.The technique developed in this work can improve the efficiency of screening for illegally added chemicals and expand the applications of IMS for detecting various chemicals in complex matrices,such as cosmetics.
作者
薛高旭
王沁怡
曹玲
孙晶
杨功俊
冯有龙
方方
XUE Gaoxu;WANG Qinyi;CAO Ling;SUN Jing;YANG Gongjun;FENG Youlong;FANG Fang(Jiangsu Institute for Food and Drug Control,Nanjing 210019,China;Affiliated Hospital of Nanjing University of Chinese Medicine,Jiangsu Province Hospital of Chinese Medicine,Nanjing 210029,China;School of Pharmacy,China Pharmaceutical University,Nanjing 211198,China)
出处
《色谱》
CAS
CSCD
北大核心
2022年第12期1119-1127,共9页
Chinese Journal of Chromatography
基金
江苏省高层次卫生人才“六个一工程”拔尖人才项目(LGY201810)
江苏省食品药品监督管理局科研项目(20170202)
江苏省市场监督管理局科技计划项目(KJ207560).
关键词
固相萃取
离子迁移谱
抗菌药物
祛痘化妆品
快速筛查
solid-phase extraction(SPE)
ion mobility spectrometry(IMS)
antibacterial drugs
anti-acne cosmetics
rapid screening
