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Determination of 15 kinds of PAHs in food using QuEChERS coupled to HPLC-FLD analysis

Application Introduction

Polycyclic aromatic hydrocarbons (PAHs) are volatile hydrocarbons produced by incomplete combustion of organic matter such as coal, petroleum, wood, tobacco, organic macromolecule compounds and are important environmental and food contaminants.

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Introduction

Polycyclic aromatic hydrocarbons (PAHs) are volatile hydrocarbons produced by incomplete combustion of organic matter such as coal, petroleum, wood, tobacco, organic macromolecule compounds and are important environmental and food contaminants. So far, there have been more than 200 kinds of PAHs, a considerable part of which are carcinogenic, such as Benzo[a]pyrene, Benz(a)anthracene, etc. PAHs are widely distributed in the environment, and can be found in every corner of our lives. Places where organics are processed, discarded, burned or used are likely to produce polycyclic aromatic hydrocarbons. The International Agency for Research on Cancer (IARC) (1976) listed 94 compounds that are carcinogenic to experimental animals, of which 15 are polycyclic aromatic hydrocarbons. Since benzo [a] pyrene is the first discovered environmental chemical carcinogen, and its carcinogenicity is very strong, thus often regarded as the representative of polycyclic aromatic hydrocarbons. It also accounts for 1% - 20% of all carcinogenic polycyclic aromatic hydrocarbons.

Experimental

Sample Preparation

Rice sample

Transfer 2 g sample and 10 mL n-hexane into a 50mL centrifuge tube, vortex for 30s, sonicate under 40 °C bath for 30 min, centrifuge at 4500 rpm for 5 min, extract supernatant into a 40 mL glass bottle. Dissolve the residue by adding another 10mL n-hexane and combine the two supernates. Blow down to nearly dryness at 35 ℃.

Chicken sample

Transfer 2 g sample and 1 g diatomite (alkaline) into a 50 mL centrifuge tube, shake with glass rod. Add 10 mL n-hexane, vortex for 30s, and sonicate under 40 °C bath for 30 min, centrifuge at 4500 rpm for 5 min. Transfer the supernatant into a 40 mL glass bottle. Dissolve the residue by adding another 10 mL n-hexane and combine the two supernates. Blow down to nearly dryness at 35 ℃.

Sample Cleanup

Add 4 mL acetonitrile into the above glass bottle, vortex for 30 s and transfer it into QuEChERS cleanup tube. Vortex for 30 s and centrifuge at 4500 rpm for 3 min. Aspirate of supernatant into 10mL glass volumetric tube. Dissolve the residue by adding another 2 mL acetonitrile and combine the two supernates. Blow down to nearly 1 mL and dissolve it to 1 mL by acetonitrile. Filter aliquot through 0.22 mm PTFT-Q filter followed by HPLC-FLD analysis.

Instrumentation

HPLC Column: Venusil® PAH, 5 μm, 200 Å, 4.6 × 250 mm;

Mobile phase: A: water; B: methanol;

Flow rate: 1.2 mL/min;

Column temperature: 30 °C;

Injection: 20 mL;

PMT gain: 10.

Table 1 Gradient

Time/min

A/%

B/%

0

15

85

2

15

85

6.5

1

99

15

1

99

25

0

100

35

0

100

35.1

15

85

45

15

85

Table 2 Fluorescence Wavelength Variation

Time/min

Excitation Wavelength/nm

Emission Wavelength/nm

0.0

280

324

7.5

254

350

8.0

254

400

9.0

290

460

9.5

336

376

10.5

275

385

13

305

430

27

305

500

Results and Discussion

QuEChERS for simultaneous extraction all fifteen PAHs from food is shown with excellent recoveries ranged from 70% - 105%. Chromatographic separation of the analytes using Venusil® PAH was also developed and satisfactory separation was gained with good resolution and stable retention.

Table 3 Accuracies and recoveries of 0.25 mg/kg spiked rice and chicken samples

Analytes

Rice

Chicken

Recoveries/%

CV/%

Recoveries/%

CV/%

Naphthalene

82.2

2.7

74.0

1.0

Acenaphthene

88.4

2.3

76.1

1.0

Fluorene

91.9

1.9

87.0

1.2

Phenanthrene,

91.3

0.3

88.6

2.1

Anthracene

93.6

1.6

88.0

1.5

Fluoranthene

93.3

1.5

91.5

2.3

Pyrene

90.4

2.4

96.2

3.9

Benzo (a) anthracene

92.3

1.0

89.8

2.3

Chrysene

94.2

1.1

87.9

2.5

Benzo (b) fluoranthene

94.1

0.4

100.9

6.3

Benzo (k) fluoranthene

93.0

0.4

87.9

3.0

Benzo (a) pyrene

90.4

0.4

86.7

3.3

Dibenzo (a,h) anthracene

90.9

2.1

87.1

3.3

Benzo (g,h,i) perylene

88.7

3.2

82.2

4.5

Indene (1, 2, 3-cd) pyrene

88.7

3.3

80.3

2.0

Figure 1 Chromatogram of all fifteen PAHs standard solution

Figure 2 Chromatogram of block rice sample

Figure 3 Chromatogram of 0.25 mg/kg spiked rice sample

Figure 4 Chromatogram of block chicken sample

Figure 5 Chromatogram of 0.25 mg/kg spiked chicken sample

Conclusion

This application note describes a robust method to determinate 15 kinds of PAHs simultaneously in food using simple QuEChERS coupled to HPLC-FLD analysis. Excellent method performance is demonstrated for each analyte together with good accuracies (70% - 105% recoveries) and precision (< 10% CVs) at 0.25 mg/kg spiked lever. Typical method performance results were within acceptable criteria.

Ordering Information

Products

Specification

Cat.No

QuEChERS

15   mL centrifuge tube

MS-9PA1229

Venusil®   PAH

5   μm, 200 Å, 4.6 × 250 mm

VP952505-L

Nitrogen   Evaporator

15   positions

NV15-G

Guard   Cartridge Holder

Compatible   with cartridge of 4.6 × 10 mm and 2.1 × 10 mm

SH-100

Direct-connection   Guard Cartridge

5   µm; 4.6 × 10 mm

VP950105-LS

1.5   mL vials

Screw   neck vials, 12 × 32 mm

AV1001-6

Caps   and Septa

Screw   neck cap, center hole; red silicone/ white PTEE septa, slitted

AV2200-0

Syringe   Filter

Monofilm,   13 mm, 0.22 μm

AS081320

Disposable   Needle-Free injection systems

2   mL, 100/pk

LZSQ-2ML

 

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