Latest phthalate plasticizer UPLC-MS/MS analysis method

Latest phthalate plasticizer UPLC-MS/MS analysis method

- Application of PFCs Isolator kit to solve the problem plasticizers background background interference

Zhao Jialu, Xia Xia Water Technology (Shanghai) Co., Ltd.

background

The importance of plasticizer testing is well known, but the biggest problem and trouble for users who currently use LC or LC/MS to detect plasticizers is that there are several of the 17 illegally added plasticizers specified by the Ministry of Health (such as DBP, DIBP, DEHP, DNOP, DINP, etc.) The background interference is very high. Due to the ubiquitous plasticizer in the environment and the interference from the analysis system itself, sometimes the background is as high as hundreds of ppb, resulting in the inability to qualitatively and quantitatively sample the plastic. Chemical agent.

Analytical method

Experimental condition

UPLC/Xevo TQD with PFCs Isolator kit

Column: BEH Phenyl 1.7μm 2.1x100mm

Injection volume: 2μL

Column temperature: 50 ÌŠC

Flow rate: 0.5ml/min

Mobile phase: A: 0.1% aqueous formic acid B: 0.1% formic acid acetonitrile solution

Mass spectrometry parameter

Ionization mode: ESI+

Electrospray voltage: 3.2kv

Desolvation gas temperature: 400 ÌŠC

Ion source temperature: 150 ÌŠC

Desolvent gas flow rate: 650L/hr

Experimental result

In the general analysis, we found that due to the high system background of plasticizers (such as DBP, DIBP, DEHP, DNOP, etc.), accurate qualitative and quantitative work could not be performed. The UPLC system equipped with PFCs Isolator kit can completely separate the interference plasticizer in the system background from the target plasticizer analyte in the sample to ensure the accuracy of qualitative and quantitative analysis results.

Figure 1. TIC diagram of plasticizer standard analysis.

Figure 2. TIC plot analysis of DIBP.

PICs ( child ion confirmation scan function ) qualitative confirmation of background interference

Using the PICs function of the Xevo series of mass spectrometers and the TargetLynx software in MassLynx, the PICs mass spectra of the actual samples collected can be compared with the standard PICs reference mass spectra, and the values ​​calculated by software-based Forward Fit and Reverse Fit values ​​can be quantified. The matching degree of the sample and the standard is judged to achieve qualitative confirmation.

Figure 3. PICs matching results for DIBP background interference

Taking DBP as an example, the qualitative confirmation function using PICs is very good. It is verified that the DBP in the system background has completely separated from the DBP chromatogram in the sample.

in conclusion

The method solves the problem of background interference of the plasticizer system, and makes the background interference completely separated from the target plasticizer analyte, and also achieves the baseline separation effect for the DBP and DIBP isomers, ensuring the quantification thereof. Accuracy and accuracy are accurate. Using the unique PICs function of the Xevo series of mass spectrometers, the MRI quantitative peaks are obtained while obtaining the product ion confirmation scan results, and the qualitative ability is extended.