A method based on in-syringe dispersive solid phase extraction (IS-D-SPE) and ultra performance liquid chromatography Orbitrap high resolution mass spectrometry for the multiresidue analysis of 117 pesticides in tea was developed. Full scan mode was acquired over an m/z range of 100–800 with Orbitrap resolution at 70000, followed by full scan/dd-MS² mode for confirmation. The identification criteria of retention time and mass accuracy tolerance was ±0.20 min and ±5.0 ppm, respectively. MS/MS fragment ions obtained dd-MS² were necessary to identify the pesticides with the same molecular mass weight. The IS-D-SPE technique involved a mixture of 200 mg PSA, 100 mg C18, and 15 mg multiwalled carbon nanotubes for the cleanup of tea matrix. Good linearity (R² > 0.99) for 117 pesticides was obtained. Satisfactory recoveries in the range of 70–120% were obtained for 105 pesticides, while intraday and interday precisions were below 20%. Limits of quantification were generally 10 μg kg^–1. Finally, this method was employed to analyze 117 pesticides in 70 tea samples.

中文翻译：

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超高效液相色谱Orbitrap高分辨率质谱和注射器内分散固相萃取快速测定茶叶中农药残留的多残留方法

建立了一种基于注射器内分散固相萃取（IS-D-SPE）和超高效液相色谱Orbitrap高分辨率质谱法对茶叶中117种农药进行多残留分析的方法。在100/800的m / z范围内获得了全扫描模式，Orbitrap分辨率为70000，然后进行了全扫描/ dd-MS ²模式进行确认。保留时间和质量准确度公差的鉴定标准分别为±0.20 min和±5.0 ppm。获得dd-MS ^2的MS / MS碎片离子是鉴定相同分子量的农药所必需的。IS-D-SPE技术涉及200 mg PSA，100 mg C18和15 mg多壁碳纳米管的混合物，用于清洁茶基质。获得了117种农药的良好线性（R ² > 0.99）。105种农药的回收率在70％至120％之间，而日内和日间的准确度均低于20％。定量限通常为10μgkg ^–1。最后，该方法用于分析70个茶叶样品中的117种农药。