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Broad screening, identification and quantitation of banned organic chemicals in cosmetics using UPLC-Q-Orbitrap high resolution mass spectrometry combined with accurate mass database and spectral library search strategy

Broad screening, identification and quantitation of banned o...

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第21届全国色谱学术报告会及仪器展览会

作者： Xianshuang Meng Qiang Ma Hua Bai Chinese Academy of Inspection and Quarantine

Broad screening, identification and quantitation of 100 multi-class organic chemicals（ninteen quinolones, four nitrofurans, three chloramphenicols, thirteen nitroimidazoles, forty glucocorticoids, nine androgens, eight progestins and four antifungal drugs） banned in cosmetics was achieved in a robust and highly sensitive and selective manner using ultra-high performance liquid chromatography-hybrid quadrupole orbitrap high resolution mass spectrometry（UPLC-Q-Orbitrap HRMS）. Ultrasonic-assisted extraction（UAE） and dispersive solid phase extraction（dSPE） were employed for sample extraction and clean-up, *** exhaustive extraction and effective purification, the samples were analyzed using the UPLC-Q-Orbitrap HRMS under full scan and data-dependent MS/MS（full scan/dd-MS2）acquisition mode. The LC-MS results were compared with an accurate mass database（including compound name, chemical formula, the m/z of precursor ion, isotopic pattern,retention time, characteristic fragment ions） and MS/MS spectral library（the entire MS/MS spectra of 100 chemcial standards） self-built with TraceFinder Software. Screening and identification were realized by comparing five key LC-MS parameters（m/z, retention time,isotopic pattern, fragment ions, and MS/MS spectra） of the samples with the database and library. Quantitation was carried out using external standardization and matrix-matched calibration curves. The whole methodology was comprehensively evaluated and validated in terms of limits of detection（LODs）, limits of quantitation（LOQs）, linearity, stability, accuracy,matrix effect and the analysis of spiked and real samples. The present UPLC-Q-Orbitrap full MS/dd-MS2 along with accurate mass database and spectral library search strategy showed great potential for high-throughput, sensitive, and reliable screening, identification, and quantitation of multi-class banned organic chemicals in routine monitoring programs of cosmetics.

关键词： Banned organic chemicals UPLC-Q-Orbitrap HRMS accurate mass database MS/MS spectral library Cosmetics

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Simultaneous Screening of 733 Pesticide Residues in Fruits and Vegetables by a GC/LC-Q-TOFMS Combination Technique

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Engineering 2020年第4期6卷 432-441页

作者： Guofang Pang Qiaoying Chang Ruobin Bai Chunlin Fan Zijuan Zhang Hongyuan Yan Xingqiang Wu Chinese Academy of Inspection and Quarantine Beijing 100176China College of Chemistry and Environmental Science Hebei UniversityBaoding 071002China Beijing Uni-Star Inspection Technology Co.Ltd. Beijing 100176China

In this paper,we report the construction of two accurate mass databases and the development of a combination detection method that simultaneously screens for 733 pesticide and chemical contaminant multi-residues via high-throughput liquid chromatography(LC)-and gas chromatography(GC)-quadru pole-time-of-flight mass spectrometry(Q-TOFMS).This work demonstrates that electronic mass spectral standards may replace chemical-source standard materials as references through one sample preparation and the combination of GC/LC-Q-TOFMS *** cutting-edge technique has also replaced multiresidue determination using targeted detection with non-targeted *** pesticide residue types,sensitivity,recovery,and reproducibility of this combination technique are evaluated in eight fruit and vegetable *** technique shows three advantages:①In comparison with the discovery capability of a single technique,the combination technique shows an improvement of 51.1%(GC-QTOFMS)and 39.6%(LC-Q-TOFMS),respectively;②the combination technique can satisfy a screening limit lower than 10μg·kg^-1 and meet the requirements of“uniform standards,”although some of the pesticide residues could be optimized to further improve screening sensitivity;③over 488 pesticides with recoveries between 60%-120%and relative standard deviation(RSD)<20%at a spiked level of 10μg·kg^-1 were detected with the combination technique in eight different *** 2012 to 2017,this combination technique was applied in an investigation to screen pesticide residues from 1384 sampling locations for 38138 batched samples covering 18 categories and 134 types of fruits and vegetables obtained from across the mainland of *** statistical analysis,533 pesticides in 115891 determinations were detected,and the regularity of pesticides in the fruits and vegetables sold on the Chinese market was shown.

关键词： Pesticide multi-residues GC-Q-TOFMS LC-Q-TOFMS accurate mass database Spectra library Fruits and vegetables

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