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Determination of 15 kinds of PAHs in oil

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 Extraction

Transfer 1 g sample into a 50 mL centrifuge tube. Add 20 mL acetonitrile and 10 mL n-hexane solution of saturated acetonitrile, vortex for 30s, and sonicate under 40 °C bath for 30 min. Refrigerated centrifugation (-4℃) at 4500 rpm for 5 min. Another 20 mL acetonitrile is added into the centrifuge tube for another extraction according to the above process. The two extracting solutions are mixed in the heart-shaped bottle, 35 °C vacuum rotary evaporation till near dry. Add 5 mL n-hexane, vortex for 30 s.

Sample Phase Extraction

Condition: 5 mL dichloromethane and 10 mL n-hexane;

Load sample: apply the sample on the cartridge. Transfer 5 mL n-hexane into aforesaid heart-shaped bottle and pour it into the cartridge. Collect the two eluents in 20 mL glass vial.

Elution: aspirate 8 mL of  dichloromethane: n-hexane (1:1, V/V); collect the eluent and combine the extract in the glass vial.

Blow down to nearly 1 mL and dissolve residue to a certain volume of 1 mL using acetonitrile, shake well. Filter aliquot through 0.22 mm PTFT-Q filter followed by HPLC-FLD analysis.

The SPE process was operated automatically by Qdaura® Automatic SPE System.

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

26

305

500

Results and Discussion

Solid phase extraction for simultaneous extraction all fifteen PAHs from oil is shown with excellent recoveries ranged from 60% - 100%. Chromatographic separation of the analytesusing Venusil® PAH was also developed and satisfactory separation was gained with good resolution and stable retention.

Table 3 Accuracies and recoveries of 0.5 mg/kg spiked oil samples

Analytes

Recoveries/%

CV/%

Naphthalene

64.7

6.7

Acenaphthene

60.4

3.5

Fluorene

83.6

1.6

Phenanthrene,

95.4

0.3

Anthracene

85.1

0.5

Fluoranthene

85.5

0.3

Pyrene

82.4

0.2

Benzo (a) anthracene

81.3

1.4

Chrysene

81.0

0.4

Benzo (b) fluoranthene

90.8

7.3

Benzo (k) fluoranthene

78.8

0.5

Benzo (a) pyrene

75.2

1.4

Dibenzo (a,h) anthracene

75.6

2.1

Benzo (g,h,i) perylene

68.9

3.6

Indene (1, 2, 3-cd) pyrene

69.7

1.7

Figure 1 Chromatogram of all fifteen PAHs standard solution (0.5 mg/mL)

Figure 2 Chromatogram of block oil sample

Figure 3 Chromatogram of 0.5 mg/kg spiked oil sample

Conclusion

This application note describes a robust method to determinate 15 kinds of PAHs simultaneously in oil using simple SPE procedure coupled to HPLC-FLD analysis. Excellent method performance is demonstrated for each analyte together with good accuracies (60% - 100% recoveries) and precision (< 10% CVs) at 0.5 mg/kg spiked lever. Typical method performance results were within acceptable criteria.

Ordering Information

Products

Specification

Cat.No

Cleanert   Florisil

500   mg/3 mL

FS5003

Venusil®   PAH

5   μm, 200 Å, 4.6 × 250 mm

VP952505-L

Qdaura®   Automatic SPE System

4   channels, 24 positions

SPE-40

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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