Institute of Food Safety, Chinese Academy of Inspection & Quarantine, Beijing 100176, China; School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China.
Institute of Food Safety, Chinese Academy of Inspection & Quarantine, Beijing 100176, China.
Anal Chim Acta. 2017 Jan 15;950:98-107. doi: 10.1016/j.aca.2016.11.006. Epub 2016 Nov 11.
A simple and universal analytical method based on ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for high throughput screening of 21 bisphenols, bisphenols digycidyl ethers and their derivatives in dairy products was developed. Response Surface Methodology (RSM) was used to optimize sample preparation conditions based on a quick, easy, cheap, effective, rugged and safe (QuEChERS) method. The analytes were extracted by using 15 mL acetonitrile with 1% acetic acid, and the extracts were further purified by using 190 mg of C18 and 390 mg of PSA. The extracts were analyzed by UHPLC-MS/MS with electrospray ionization (ESI) source. Linearity was assessed by using matrix-matched standard calibration and good correlation coefficients (r > 0.99) were obtained. The limits of quantitation (LOQs) for the analytes ranged from 0.02 to 5 μg kg. The extraction recoveries were in a range of 88.2%-108.2%. Good method reproducibility in terms of intra- and inter-day precision was observed, yielding relative standard deviations (RSDs) less than 8.9% and 9.9%, respectively. The validation method results revealed that the proposed method was sensitive and reliable. Finally, this method was successfully applied to dairy product analysis.
建立了一种基于超高效液相色谱-串联质谱法（UHPLC-MS/MS）的简单通用分析方法，用于高通量筛选乳制品中的 21 种双酚、双酚二缩水甘油醚及其衍生物。响应面法（RSM）用于根据快速、简便、廉价、有效、耐用和安全（QuEChERS）方法优化样品制备条件。使用 15 mL 含 1%乙酸的乙腈提取分析物，并用 190 mg C18 和 390 mg PSA 进一步纯化提取物。采用电喷雾电离源（ESI）的 UHPLC-MS/MS 进行分析。通过基质匹配标准校准评估线性，得到良好的相关系数（r>0.99）。分析物的定量限（LOQs）范围为 0.02-5μg/kg。萃取回收率在 88.2%-108.2%范围内。日内和日间精密度方面的方法重现性良好，相对标准偏差（RSD）分别小于 8.9%和 9.9%。验证方法结果表明，该方法灵敏可靠。最后，该方法成功应用于乳制品分析。
