Rapid And Direct Determination Of Phthalate Acid Esters In Liquors And Milk Using Air Flow Assisted Reactive Extractive Electrospray Tandem Mass Spectrometry

As an industrial additive, Phathalic acid esters(PAEs) were mainly used as the plasticizer in a broad range. However, plasticizers can influence the body secretion system with reproductive ability weakened for male and precocious puberty for females; what’s more, it may influence embryonic development through the placenta lipid and zinc metabolism, causes the slow growth of embryo, even to carcinogenicity. So it is imperative to strengthen the study of plasticizer. Current analytical techniques routinely include some concentration pretreatment methods, such as solid-phase extraction(SPE), solid-phase microextraction(SPME), and dispersive liquid-liquid microextraction(DLLME) and so on, coupled with gas chromatography(GC), high performance liquid chromatography(HPLC), or GC-mass spectrometry(MS) and HPLC-MS. These methods can offer satisfactory sensitivity and good reproducibility, and were regard as the routine method for PAEs detection in various matrixes. However, these methods are time-consuming(> 40 min) with laborious sample pretreatment, even expensive and not environmentally friendly. Herein, air flow assisted extractive electrospray ionization, termed as air flow assisted reactive extractive electrospray(AFAEESI), was developed. Combined with Q-TOF tandem mass spectrometry, AFAEESI tandem mass spectrometry(MS/MS) was established and used for the directly continuous analysis of PAEs in liquors and milk, and got the following achievement: 1、Developed an air flow assisted extractive electrospray ion source with satisfactory sensitivity, good reproducibility, easy to operate, and combined with Q-TOF mass spectrometry, the AFAEESI-MS/MS can be used to directly analyze the compounds in different solutions. 2、AFAEESI-MS/MS was used to directly analyze four phthalatic acid esters(PAEs) in liquor. The limits of detection(LODs) and limits of quanti?cation(LOQs) were in the range of 0.011-0.035 and 0.038-0.087μg m L-1, respectively. Very good linearies varied in the range of 0.035-10mg m L-1 with the correlation coef?cients of 0.9758-0.9990. The precisions of the method were 2.1-4.4 in terms of RSD% and the recoveries were 89.3-102.7%. 3、AFAEESI-MS/MS was used to directly analyze four phthalatic acid esters(PAEs) in milk. The limits of detection(LODs) and limits of quanti?cation(LOQs) were in the range of 0.023-0.139 and 0.077-0.464μg mL-1, respectively. Very good linearies varied in the range of 0.01-10μg mL-1 with the correlation coef?cients of 0.9837-0.9979. The precisions of the method were 1.9-5.7 in terms of RSD% and the recoveries were 89.3-102.7%.based on triplicate measurements.