- Phone
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Address
No. 2466 Science and Technology Avenue, Lin'an District, Hangzhou City, Zhejiang Province, China
Solution
Hangzhou Puyu Technology Development Co., Ltd
01 Background
Phthalates (PAEs), also known as phthalates, are plasticizers widely used in the production and manufacturing of various plastic products. Their main function is to increase the flexibility and processability of plastics. However, PAEs are environmental hormones that can disrupt the balance of the human endocrine system, posing a potential threat to health. In June 2011, the National Health Commission of China issued Announcement No. 16, which included PAEs in the list of non edible substances that may be illegally added to food and food additives that are prone to abuse, and explicitly prohibited their direct use in food production.
02 Pu Yu Technology Solution
To effectively detect the content of PAEs in food, this plan refers to the "National Food Safety Standard for Determination of Phthalates in Food" (GB 5009.271-2016) and uses gas chromatography-mass spectrometry to analyze 18 PAEs in food. This scheme is stable and reliable, with high sensitivity and excellent linearity, and can accurately perform qualitative and quantitative detection of PAEs in food.
03 Instruments and equipment
Gas chromatography-mass spectrometry (EXPEC 3750 GC-MS, Hangzhou Puyu Technology Development Co., Ltd.)
04 Test Method
·Standard sample:Withn-hexaneAs a solvent, use the stepwise dilution method to dilute diisononyl phthalate（DINP）Prepare a standard series solution of 0.5~20.0 μ g/mL, and prepare the remaining 17 PAEs into a standard series solution of 0.02~1 μ g/mL.
·Instrument parameters: The reference conditions for the EXPEC 3750 gas chromatography-mass spectrometer are shown in the table below.
Reference conditions for gas chromatography-mass spectrometry
05 Results and Discussion
Referring to the instrument conditions, detection and analysis were carried out on 18 PAEs substances, and all target substances were able to achieve good baseline separation. Figures 1 and 2 show the total ion chromatogram and DINP characteristic ion chromatogram of 18 PAEs substances, respectively.
Figure 1 Total ion chromatogram of 18 PAEs substances
注： 1-DMP； 2-DEP； 3-DAP； 4-DIBP； 5-DBP； 6-DMEP； 7-BMPP； 8-DEEP； 9-DPP； 10-DHXP； 11-BBP； 12-DBEP； 13-DCHP； 14-DEHP； 15-DPhP； 16-DNOP； 17-DINP； 18-DNP
Figure 2 DINP characteristic ion flow chromatogram (m/z=127)
06 Standard Curve
According to the experimental method, the external standard method is used for quantification. The results showed that the linear correlation coefficient R2 of all PAEs was greater than 0.999, indicating good linearity. The standard curve fitting diagram of some PAEs substances is shown in Figure 3, and the specific data is shown in the table below.
Figure 3: Standard Curve Fitting of Partial PAEs
Precision and detection limit of method 07
Conduct high and low concentration precision testing based on the concentration gradient of each PAEs substance standard sample in the experimental method. The results showed that the precision of high concentration ranged from 0.48% to 1.59%, while the precision of low concentration ranged from 0.93% to 6.50%. The instrument method had good precision.
Conduct experiments on the detection limits of 18 PAEs in the method using blank matrix samples. The results showed that the detection limit of DINP was 408.25 μ g/kg, while the detection limits of the other 17 PAEs ranged from 5.92 μ g/kg to 16.93 μ g/kg.
Summary Table of Methodological Analysis Results for 18 PAEs Substances
08 Actual Sample Analysis
According to the requirements of the national food safety standard "Determination of Phthalates in Food" (GB 5009.271-2016), weigh 1.0 g of soy sauce A, add 4 mL of distilled water, vortex and mix well, accurately add 10 mL of n-hexane, continue to vortex for 1 minute, vigorously shake for 1 minute, extract by ultrasound for 30 minutes, centrifuge at 1000 r/min for 5 minutes, take the supernatant, and perform GC-MS analysis.Through processing and analysis of soy sauce A, the results showed that all 18 PAEs in soy sauce A were below the detection limit of the method.
Conclusion 09
The EXPEC 3750 gas chromatography-mass spectrometer was used to analyze 18 PAEs in soy sauce (food), with a linear correlation coefficient R2 ranging from 0.9991-0.9998, high concentration precision ranging from 0.48% to 1.59%, and low concentration precision ranging from 0.93% to 6.50%. The detection limit of DINP is 408.25 μ g/kg, while the detection limits of the other 17 PAEs range from 5.92 μ g/kg to 16.93 μ g/kg. Analysis of 18 PAEs in soy sauce showed no detection. This scheme has good precision and detection limit, and can provide reliable technical support for the detection of PAEs in food.