Determination of human pharmaceutical and synthetic hormones in STPs effluents

along Selangor River and Klang River

Mohamad Pauzi Zakaria

Mustafa Ali

and

Najat Ahmed AL-odaini

Pharmaceuticals are:

Biologically active compounds Covers a complex class of widely used

compounds as human and veterinary medicine, in agriculture and aquaculture

Exposed to the environment with very little attention

They received little attention because they are not regulated as environmental pollutants

Pharmaceuticals, bioactive Pharmaceuticals, bioactive natural wastes and known toxic natural wastes and known toxic compoundscompounds

Pharmaceuticals : Chloramphenicol, sulphonamides

Bioactive natural wastes: Estrogens

Known toxic compounds: Paraquat

POPS

General analytical technique used in pharmaceutical analysis in aqueous

environmental matrices

(1 liter water sample) and Storage at 4 ºc

filtration to remove particulate mater

Analysis using LC/MS/MS

Extraction using solid phase extraction (MCX)

Sample pretreatment (Add Na2EDTA/HCl)

Three main steps in the analytical technique must be optimized in the following order:

1. MS/MS Parameters2. LC method 3. Solid phase extraction

Method development and optimization

Example :Lovastatin

M.W

Ionization source

Precursor ion

D.I CE Parent ion scan

MRMTransitio

n

404. ESI +ve 405.6 285.5173.4225.4199.5

8251820

All ions are real

405.6 >285.5 173.4 225.4 199.5

Selangor RiverSelangor River

Klang RiverKlang River

Klang RiverKlang RiverKlang River in September

3.36

4.23

3.11

0

1

2

3

4

5

6

IK 0

1

IK 0

2

IK 0

3

IK 0

4

IK 0

5

IK 0

6

IK 0

7

IK 0

8

IK 0

9

IK 1

0

IK 1

1

IK 1

2

IK 1

3

IK 1

4

IK 1

5

IK 1

6

IK 1

7

IK 1

8

IK 1

9

IK 2

0

IK 2

1

IK 2

2

IK 2

3

IK 2

4

Sample

Co

nce

ntr

atio

n (

pp

t)

ESTRONE

ESTRADIOL

Klang River in January

2.93 2.80

0

1

2

3

4

5

6

IK 0

1

IK 0

2

IK 0

3

IK 0

4

IK 0

5

IK 0

6

IK 0

7

IK 0

8

IK 0

9

IK 1

0

IK 1

1

IK 1

2

IK 1

3

IK 1

4

IK 1

5

IK 1

6

IK 1

7

IK 1

8

IK 1

9

IK 2

0

IK 2

1

IK 2

2

IK 2

3

IK 2

4

Sample

Co

nce

ntr

atio

n (

pp

t)

ESTRONE

ESTRADIOL

Klang River in November

2.74 2.74

0

1

2

3

4

5

6

Sample

Co

nce

ntr

atio

n (

pp

t)

ESTRONE

ESTRADIOL

Levels of Estrone and Estradiol in Waste Water Samples

228.

5

15.0

116.

0

44.3

7.1

53.4 57.4

78.4 84

.2

5.48

26.1

7

71.8

671

84.7

9

92.5

5

176.

17

170.

14

4.5

4.9

5.4 7.3

5.2

44.5

5

0.0

50.0

100.0

150.0

200.0

250.0

1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31 33 35 37 39 41 43 45 47 49 51 53 55

Con

cent

ratio

n (p

pt)

Estrone

Estradiol

Selangor RiverSelangor RiverSelangor River in October

0

1

2

3

4

5

6

Sample

Co

nce

ntr

atio

n (

pp

t)

ESTRONE

ESTRADIOL

Selangor River in December

0

1

2

3

4

5

6

ISR 01 ISR 02 ISR 03 ISR 04 ISR 05 ISR 06 ISR 07 ISR 08 ISR 09

Sample

Co

nce

ntr

atio

n (

pp

t)

ESTRONE

ESTRADIOL

Thank You for Your Kind Attention