分析测试学报2024，Vol.43Issue(7)：1003-1010,8.DOI:10.12452/j.fxcsxb.24042401
mPFC-QuEChERS净化联合UPLC-MS/MS法快速测定3种根茎类中药材中16种真菌毒素
Determination of 16 Mycotoxins in Three Radix and Rhizome Chi-nese Herbal Medicines by mPFC-QuEChERS with UPLC-MS/MS
摘要
Abstract
A method was established using a rapid multiple filtrate purification column(mPFC-QuEChERS)combined with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)for the simultaneous determination of sixteen mycotoxins in three radix and rhizome Chinese herbal medicines.Through optimization of the liquid chromatography conditions,mass spec-trometry conditions,and sample pretreatment process,the sample was extracted with a high-speed homogenizer using an 80％acetonitrile solution(containing 2％acetic acid),and single-step purified by a mPFC-QuEChERS purification column.The analytes were separated by a shim-pack Velox PF-PP chromatographic column,and eluted with a gradient of 0.01％formic acid/0.2 mmol/L formic ac-id ammonium solution and methanol as the mobile phase,and determined in positive and negative electrospray ionization mode in multiple reaction monitoring(MRM)mode.Quantitative analysis was performed using the external standard method.Under the optimal experimental conditions,sixteen mycotoxins showed good linear relations in their mass concentrations(r＞0.99),with the detection limits(LODs)ranging from 0.3 to 25 μg/kg and quantification limits(LOQs)ranging from 0.5 to 50μg/kg.The residual levels of 16 mycotoxins were spiked at 2.5,10 and 20 times of LOQ with aver-age recoveries ranging from 63.3％to 110％and relative standard deviations(RSDs)ranging from 0.20％to 6.7％.60 batches of Chinese herbal medicines were detected,and the detection rate was 30％.Ochratoxin A(OTA),15-acetyldeoxynivalenol(15-ACE)and sterigmatocystin(ST)were rela-tively high detected.Notably,OTA was detected in 9 batches of Astragali Radix and 2 batches of Co-donopsis Radix,representing the highest detection rate.The method was simple,high sensitive,and practicable,which can be used for the rapid screening and quantitative analysis of 16 mycotoxins in radix and rhizome Chinese herbal medicines.关键词
真菌毒素/快速滤过型净化柱/超高效液相色谱-串联质谱法/根茎类中药材Key words
mycotoxins/mPFC-QuEChERS/UPLC-MS/MS/radix and rhizome Chinese herbal medicines分类
化学化工引用本文复制引用
谢思敏,古锶巧,顾利红,栗建明..mPFC-QuEChERS净化联合UPLC-MS/MS法快速测定3种根茎类中药材中16种真菌毒素[J].分析测试学报,2024,43(7):1003-1010,8.基金项目
广东省科技创新战略专项资金(20212210005) （20212210005）
