GC-MS方法

μ

L10

μ

g/mL of C

30

-

ββ

-hopaneand

100

μ

L10

μ

< br>g/mL of terphenyl-d

14

for TPH, biomarker andPAHs analysis,

respectively), and then adjusted to an accurate preinjection volume of

1.00 mL for GC

–

MS and GC-FID analyses.

Agilent 6890 GC equipped with an Agilent 5973 massselective

detector (MSD). System control and data acquisition wereachieved with

an Agilent G1701 BA MSD ChemStation. The GC separation was

achieved using an HP-5MS fused silica capillary column(30 m×

0.25 mm

id, 0.25

μ

m film thickness) with different temperature programs for

specific target compounds. Samples wereinjected in splitless mode. The

carrier gas was heliumat 1.0 mL/ injector, MSD transfer line, and

ion source temperatures wereset at 290, 280, and 230

℃

, respectively. The

MSD was performedin the selected ion monitoring (SIM) mode. The

concentrationsof the individual PAH, normal alkanes and biomarker

compoundswere determined based on the internal standards

d

14-

-androstane and C30-

ββ

-hopane

, respectively.

4.

Solid waste deposits as a significant source of contaminants of

emerging concern tothe aquatic and terrestrial environments

—

A

developing country case study fromOwerri, NigeriaAugustine

ArukweScience of the Total Environment(

小二大二

)

Solid phase extraction (SPE) using OASIS HLB sorbent

(Waters)was applied to extract the water sample afterfiltration (45 μm

glass

Fiberfilter). From the 820 mL water sample, 43 mg (dry weight)particles

werefiltered which were not analyzed separately. The SPEprocedure was

performed in accordance withRocha et al. (

2011

All target EDCs were

extracted, from both fortified water matrices and real water samples,by

solid phase extraction (SPE) using OASIS HLB cartridges adapted in an

off- line SPEvacuum extraction device (Waters). The breakthrough

volume, pH adjustment, washesand elution conditions followed a method

initially developed to extract phenoliccompounds and steroids in water

16Optimisation of derivatisation for the analysis of estrogenic

compounds inwater by solid-phase extraction gas

c hromatography

–

mass spectrometry

小二大二

The target compounds were extracted from water samplesby SPE

technique. One hundred nanogram of E1, E2, EE2,16

α

-hydroxyestrone,

4-nonylphenol, bisphenol A, and 4-tertoctylphenol were spiked (in

triplicate) in 500 mL of ultrapurewater for the recovery test. The Oasis

SPE cartridges (0.2 gHLB, Waters) were conditioned with 5 mL of ethyl

acetate toremove residual bonding agents, followed by 5 mL of

methanolwhich was drawn through the cartridges under very low

vacuumto ensure that the sorbents were soaked in methanol for 5

ultrapure water (3×

5 mL) was passed through the cartridges at

a rate of 1

–

2 mL min

?

1

.Water samples were extractedat

a ?ow rate less

than 5 mL min

?

1

，

except when the effect of

?

ow rate on EDC recovery

was studied. The cartridges weredried under vacuum and then the

analytes were eluted to vials(20mL) from the sorbents with 10 mL of

ethyl acetate at a ?owrate of 1 mL min

?

1

. The solvents were blown down

to 1 mL

under a gentle ?

ow of nitrogen at less than 50

℃

. In addition,the

effects of water properties such as the presence of aquatic colloids and

surfactants on EDC recovery were assessed by spikingdifferent amount of

colloids and surfactants to test samples. Themethod developed was

further ve

ri?ed by checking recoveries in

natural matrices, where river

w

ater and sewage ef?uent samples

(1 L) were

?

ltered through

pre-combusted

GF/F ?lters (0.7 μm)

and spiked with 50

–

500 ng of the

target EDCs. These sampleswere then extracted using SPE and analysed

by GC

–

MS.]. In this study, the last method was broadened forthe analysis

of 4-OP and alkylphenolethoxylates (NP1EO, NP2EO, OP1EO,

OP2EO).Briefly, the condition step was carried out with 5 mL of ethyl

acetate, to remove residualbonding agents, followed by 5 mL of methanol

and 3

×

5 mL of ultrapure water, at a flowrate of 1mL min

-1

. Spiked water

samples and surface water matrices (500 mL) added withthe above

referred IS, were loaded onto SPE cartridges at a constant flow rate of5

mL min

-1

followed by a washing step with 10 mL of ultrapure water and

methanol (9:1).Cartridges were dried under vacuum for 30 min and then

eluted with 10 mL of ethylacetate, at 1 mL min

-1

. The resulting extracts

were evaporated to dryness in a heatingblock at 40

℃

under a gentle

stream of nitrogen and reconstituted in 500mL of anhydrousmethanol.).

Briefly, before the 820 mL-water sample was extracted by SPE,

theinternal standards,4-n-nonylphenol and estradiol diacetate (200 ngeach)

were added and the SPE cartridge was conditioned using5 mL of

methanol and 5 mL of pure water. After sample loading at3 mL/min, a

wash step using 3 mL of water (10% methanol) wasperformed and

thereafter, 12 mL ethylacetate was applied for resulting

extract was evaporated to dryness and reconstituted toafinal volume of 1

mL using cyclohexan

e, from which an aliquot of 1μL

was analyzed by gas