1. Application Range

It is suitable for the determination of oil phthalate compounds (rapeseed oil is used as sample matrix in this experiment).

Reference: SN/T 3147-2017 Determination of Phthalate Estates in Exported Foods

2. Extraction Steps

1) take 5 g samples in glass tube, add 2 mL acetonitrile saturated n-hexane, mix with vortex , then add 4 n-hexane saturated acetonitrile. Mix by vortex, ultrasound for 10 min, centrifuge for 5 min (3000r/ min), carefully transfer the lower layer solution to another glass tube; Add 4 n-hexane saturated acetonitrile, repeat extraction once and combine two extracts.

2) Put extract in 40℃ water bath to dry, accurately add 5 mL acetonitrile and mix by vortex. Add it in Welchrom®QuEChERS purification tube (P/N:00533-20020), mix by vortex, centrifuge for 5 min (3000r/) and take the supernatant to be tested.

3. Chromatographic Conditions

 3.1 GC Conditions

 Column: WM-5MS,30m*0.25mm*0.25μm

 Injection inlet temperature: 260℃

 Temperature program: initial column temperature 60℃, maintain 1 min; rise at 20℃/ min to 220℃, maintain 1 min; and then rise at 5/ min to 250, maintain 1 min; rise at 20℃/ min to 290℃, maintain 7.5 min.

 Carrier gas: high-purity helium (purity >99.999%)

 Injection way: splitless injection

 Injection volume: 1μL

3.2 MS Conditions

Ionizing method: electron bombardment ionization source (EI)

Ionizing energy :70 Ev

Transmission line temperature :280℃

Ion source temperature :230℃

(b) Monitoring: ion scanning (SIM)

Solvent delay: 7.5 min

4. Chromatogram or Result of Spike Recovery

Fig 1. Chromatogram of 0.125μg/mL mixed standards phthalate esters 

Table 1 Related Peak Information

No.ProductRetentionWidthArea
1DMP7.9950.026231015
2DEP8.840.022215986
3DIBP10.6240.026331212
4DBP11.3840.028240580
5DMEP11.730.02980356
6BMPP12.4420.055144812
7DEEP12.8070.03465897
8DPP13.1760.032149986
9DHXP15.3210.05197533
10BBP15.4980.03875616
11DBEP16.9710.03820408
12DCHP17.6690.03561322
13DEHP17.8330.03351514
14DPhP17.9820.03353156
15DNP18.830.02416379
16DNOP19.4350.02838063

Fig 2. Chromatogram of blank solvent  

Fig 3. Chromatogram of purified rapeseed oil samples

Fig 4. Chromatogram of purified rapeseed oil samples at 0.05mg/kg

Table 2. Recovery rate of spiked samples

No.NameWidthArea
1DMP91.08%4.33%
2DEP92.83%0.24%
3DIBP64.94%0.85%
4DBP84.56%2.40%
5DMEP98.81%0.47%
6BMPP94.82%4.31%
7DEEP111.22%4.07%
8DPP93.01%0.12%
9DHXP83.75%0.11%
10BBP133.48%5.74%
11DBEP138.31%1.07%
12DCHP87.88%0.42%
13DEHP75.59%4.82%
14DPhP109.14%1.41%
15DNP72.99%3.40%
16DNOP68.25%0.64%

5. Ordering Information of Related Products

P/NNameSpecification
00533-20020Purification tubeWelchrom® QuEChERS Purification tube-2ml,AOAC method,150mg MgSO4,50mg PSA,50mg C18E,used in fat and wax fruits and vegetables,100/pk
03904-22001GC columnWM-5MS, 30m*0.25mm*0.25μm

If you have any problem or require further information, please contact info@welchmat.com.


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