Zhao Yang, Araujo Magali, Flynn Thomas J, Mapa Mapa S T, Mossoba Miriam E, Sprando Robert L
Division of Toxicology (DT), Office of Applied Research and Safety Assessment (OARSA), Center for Food Safety and Applied Nutrition (CFSAN), U.S. Food and Drug Administration (U.S. FDA), Laurel, Maryland, USA.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2021 Mar;38(3):361-370. doi: 10.1080/19440049.2021.1873426. Epub 2021 Jan 22.
A routine, selective and sensitive ultra-high performance liquid chromatography-electrospray ionisation tandem triple quadrupole mass spectrometry (UHPLC-ESI-MS/MS) method was developed and validated for the quantification of 3-monochloropropane-1,2-diol (3-MCPD) in Caco-2 cell transport buffer (FaSSIF-V2, the second version of a fasted state simulated intestinal fluid) and receiving buffer (HBSS, Hank's balanced salt solution). The method involves measuring deuterated 3-MCPD (3-MCPD-) as internal standard (IS) during the entire analytical procedure to obtain precise and accurate results. The separation was performed on a Poroshell 120 HILIC column (2.7 m, 3.0 × 50 mm) at a flow rate of 0.3 mL/min using water (containing 0.025% acetic acid) and acetonitrile (containing 0.025% acetic acid) as the mobile phases. Mass spectrometric detection was operated in dynamic multiple reaction monitoring (dMRM) in negative ion mode. The method exhibited high sensitivity. The limits of detection (LOD) for 3-MCPD in FaSSIF-V2 and HBSS were 0.012 and 0.014mol/L, and the limits of quantification (LOQ) were 0.039 and 0.045 mol/L, respectively. Satisfactory results were observed for linearity (> 0.999), intra-day precision (% <7.7% in FaSSIF-V2 and <6.6% in HBSS), inter-day precision (% <5.9% in FaSSIF-V2 and <5.6% in HBSS), accuracy (% error within ± 10%), and sample stability (% <7.7% and % error within ± 10%). The method has been successfully applied to quantify 3-MCPD in Caco-2 cell transport and receiving buffers. The results were in good agreement with those obtained with gas chromatography-tandem mass spectrometry (GC-MS).
开发并验证了一种常规、选择性且灵敏的超高效液相色谱-电喷雾电离串联三重四极杆质谱法（UHPLC-ESI-MS/MS），用于定量测定Caco-2细胞转运缓冲液（FaSSIF-V2，禁食状态模拟肠液的第二个版本）和接受缓冲液（HBSS，汉克斯平衡盐溶液）中的3-一氯丙烷-1,2-二醇（3-MCPD）。该方法在整个分析过程中涉及测量氘代3-MCPD（3-MCPD-）作为内标（IS），以获得精确和准确的结果。在Poroshell 120 HILIC柱（2.7μm，3.0×50 mm）上进行分离，流速为0.3 mL/min，使用水（含0.025%乙酸）和乙腈（含0.025%乙酸）作为流动相。质谱检测在负离子模式下以动态多反应监测（dMRM）运行。该方法具有高灵敏度。FaSSIF-V2和HBSS中3-MCPD的检测限（LOD）分别为0.012和0.014μmol/L，定量限（LOQ）分别为0.039和0.045μmol/L。在线性度（>0.999）、日内精密度（FaSSIF-V2中<7.7%，HBSS中<6.6%）、日间精密度（FaSSIF-V2中<5.9%，HBSS中<5.6%）、准确度（误差百分比在±10%以内）和样品稳定性（<7.7%且误差百分比在±10%以内）方面观察到令人满意的结果。该方法已成功应用于定量测定Caco-2细胞转运和接受缓冲液中的3-MCPD。结果与气相色谱-串联质谱法（GC-MS）获得的结果高度一致。
