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24 : 401-420 2006
Ann Rept. BFDA Taiwan R.O.C. 24 : 401-420 2006

100(Cd)(Cr)(Cu)(Ni)
(Pb)(Sn)(Zn)(Hg)

(certified
reference materials) 5 mL10 mL

100
107
300.007 g/g (N.D. ~ 0.067 g/g)
0.011 g/g (N.D. ~ 0.082 g/g)0.270 g/g (N.D. ~ 1.954 g/g)
0.022 g/g (N.D. ~ 0.112 g/g)0.016 g/g (N.D. ~ 0.087
g/g)0.019 g/g (N.D. ~ 0.330 g/g)2.909 g/g
(1.097 ~ 6.366 g/g)0.188 g/g (0.001 ~ 1.515 g/g)

(2)

(3)

(1)

-401-

Ann. Rept. BFDA

100
(Cd)(Cr)(Cu)(Ni)(Pb)
(Sn)(Zn)(Hg)
(15)

(4)
(5)

(6)

(osteomalacia)
(6)

250 mg
(7)
(8)

(8)
(9)

, (6)

(10)

(5)

(11)

(12)

(13,14)

9219210

(Cadmium)(Chromium)
(Nickel)(Lead)(Tin)
(Copper)(Mercury)
1000 g/mLICP(Zinc)
(1000 g/mL)
Merck KGaA

1. (nitric acid)(
10 mg/mL-0.5 mg/mL
1.0 mg/mL-0.6 mg/mL
)
(Hg 0.005 ppm
)(stannous chloride)
(Hg 0.000001% )
(Vanadium pentaoxide)

-402-

Merck KGaA

Millipore (Beford, MA, USA)


18 m7/cm

2. ( s t a n d a r d r e f e r e n c e
material certied reference material)
(dogfish muscle, DORM-2)
(dogfish liver, DOLT-2)
(dogfish liver, DOLT-3)
National Research Council Canada
(NRCC)
! (mussel tissue)BCR477
(Commission of the European
Communities)Community Bureau of
Reference (BCR)

1. 10 mL25 mL50 mL100


mL10 mL5 L
(2 mm10
)(pyrex)

(11, v/v)

2. (THGA graphite tube)Model


B050-4033Perkin-Elmer

3.
(Hollow cathode lamp)PerkinElmer
(Hitachi)

Perkin-Elmer
! (Flame Atomic
Absorption Spectrophotometer)
Hitach
! ( M e r c u r y A t o m i c
Fluorescence SpectrometerHg-AFS)
Merlin PSA
10.025, PS Analytical, U.K
Schott SLK2Germany
! (Focused Microwave
Digester)Model Microdigest 3.6
250 WProlabo

50 ng/
mL2 ng/mL25 ng/mL10 ng/
mL100 ng/mL20 mL

0.51.01.52.0 ng/mL
246810 ng/mL
1020304050 ng/mL
510152025 ng/mL
1020304050 ng/mL
20406080100
ng/mL

228.8 nm357.9 nm
324.8 nm232.0 nm283.3 nm
286.3 nm

0.250.500.751.00 mg/

! (Zeeman
Graphite Furnace Atomic Absorption
Spectrophotometer)Perkin Elmer
4110ZL AS-72

-403-

Ann. Rept. BFDA

mL
213.9 nm

250500750 ng/L

1 g10 mL
5 mL
95 ~ 120

10 mL

1 g
10
mL2
10 mL4
30 W
1080 W35

1-210%
20 mL
50 mL

10 mL

()
10

4.5
4.5
4.5

9.0
9.0
9.0

1.

(ppm)
2.

(ppm)

15
50
60

( I D L )
(MDL)(16)
(IDL)

(MDL)

1 ~ 5

(mL/min)

4.5
9.0

-404-

(Sa)
Sa

Element

Slope

Intercept

Pb

0.0215

0.0066

0.9999

Cd

0.0224

0.0016

0.9999

Ni

0.0227

0.0029

0.9997

Cr

0.0338

0.0109

0.9999

Sn

0.0162

0.0470

0.9995

Cu

0.0480

-0.0026

0.9994

0.1521

0.0023

0.9993

111.73

-14.352

0.9998

GFAAS analyzer

(20 L)

(17)
(17)
Almeida Lima(18)Gawalko et al.(19)
Yaru et al. (20)Vaidya Rantala (14)

50017001200
13008501200
1200
230021002400
14002400

FLAAS analyzer
Zn
Hg-AFS analyzer
Hg

0.9993(r)
0.9998

Chen(13)Vaidya Rantala(14)
(450)

Vaidya Rantala(14)

(X)
(Y)

(r)0.9994 ~
0.9999(r)

-405-

Ann. Rept. BFDA

0.0001 g/mL0.0002 g/mL


0.0003 g/mL0.0012 g/mL
0.0006 g/mL0.0014 g/mL
0.002 g/mL0.00001
g/mL
2.

0.001 g/g0.004 g/
g0.003 g/g0.006 g/g
0.005 g/g0.01 g/g
0.01 g/g0.0005 g/g

(5000 mL)
2 mm

!(standard reference material)

1
g
BCR477DORM-2DOLT-2DOLT-3

10.0%

()
! ( I D L )
(MDL)
1.

9219210

Elements

Certied values
(mg/kg)

Determined a
values(mg/kg)

CV(%)

dogsh muscle

Cd

0.0430.008b

00.048 0.001

1.2

DORM-2

Cu

2.3400.12

02.236 0.017

0.8

Ni

19.403.1

17.648 1.063

6.0

Zn

25.602.3

26.333 0.243

0.9

dogsh liver DOLT-2

Cr

0.3700.08

00.343 0.014

4.1

dogsh liver

Pb

0.3190.045

00.297 0.009

3.1

DOLT-3

Hg

3.3700.14

03.337 0.087

2.6

mussel tissue BCR477

Sn

2.7 (0.328)c

02.649 0.134

5.1

Sample

aaverage of triplicate
bvalue is expressed as standard deviation.
cvalue in the parenthesis is uncertainty

-406-

()

(hairtail)

(porgy)

IDL
(mg/mL)

MDL
(mg/g)

0.0001

0.001

(Pacic saury)

Cd
Cr

0.0002

0.004

(pomfret)

Cu

0.0003

0.003

(parrotsh)

Ni

0.0012

0.006

(swordsh)

Elements
Analyzed by GFAAS

Pb

0.0006

0.005

(tuna)

Sn

0.0014

0.01

(shark)

(salmon)

(cod)

(others)

30

100

Analyzed by FLAAS
Zn

0.002

0.01

Analyzed by Hg-AFS
Hg

0.00001

0.0005

100
(hairtail)(porgy)
(Pacific saury)(pomfret)
(parrotfish)() (Swordfish)
(tuna)(shark)
(salmon)(cod)
30
0.007 g/g (N.D. ~ 0.067 g/g)
0.011 g/g (N.D. ~ 0.082 g/
g)0.270 g/g (N.D. ~
1.954 g/g)0.022 g/
g (N.D. ~ 0.112 g/g)
0.016 g/g (N.D. ~ 0.087 g/g)
0.019 g/g (N.D. ~ 0.330 g/g)
2.909 g/g (1.097 ~
6.366 g/g)0.188 g/
g (0.001 ~ 1.515 g/g) ()

1.
100()
0.023 g/g (0.006 ~ 0.046 g/g)

0.002 g/g (0.001 ~ 0.003N.D. ~ 0.007


g/g )
0.067 g/g

2.
( )
0.020 g/g (0.006 ~ 0.0460.001 ~
0.082 g/g)
0.005 g/g (0.003 ~ 0.008 g/g )

0.082 g/g
3.
1.369 g/g (0.640

-407-

-408-

30

100

porgy

Pacic saury

pomfret

parrotsh

swordsh

tuna

shark

salmon

cod

others

Total

Cd
b

0.0110.012
N.D.~0.082

N.D.~0.067

N.D.~0.046

0.001~0.067

0.0070.011

0.0090.011

0.001~0.082

0.001~0.008

0.0070.014

0.0200.029

0.003~0.027

N.D.~0.007

0.0030.003

0.0160.010

0.006~0.0180

0.002~0.033

0.0020.002

0.0100.004

N.D. C~0.044

0.0110.011

0.003~0.035

0.010 0.011
0.0120.015

0.006~0.046
b

0.006~0.046

0.0200.015

0.0230.012

N.D.~0.027

0.001~0.005

0.003~0.008
0.0070.010

0.002~0.017

0.0030.0001

0.0050.002

N.D.~0.028

0.005~0.015

0.0060.005

0.0080.010

0.003~0.0210

0.001~0.003

0.0090.003

0.0100.006

0.007~0.019

0.0140.005

Cr

0.0020.001

0.001~0.008

0.003 0.003

aaverage
bvalue is expressed as standard deviation.
cN.D. means not detected.

No.

hairtail

Variety

N.D.~1.954

0.2700.353

0.035~0.793

0.2590.181

0.079~0.132

0.1070.021

N.D.~0.387

0.1940.151

N.D.~0.208

0.1000.077

0.022~0.356

0.2230.109

0.119~0.218

0.1700.040

0.113~0.229

0.1800.047

0.047~0.139

0.1020.030

0.640~1.954

1.3690.529

0.116~0.189

0.1510.027

0.106~0.192

0.1530.027

Cu

N.D.~0.112

0.0220.022

N.D.~0.046

0.0110.009

0.012~0.053

0.0290.016

0.002~0.061

0.0360.022

0.014~0.079

0.0410.026

0.011~0.084

0.0330.028

0.004~0.052

0.0300.015

N.D.~0.046

0.0140.017

N.D.~0.043

0.0170.018

N.D.~0.112

0.0300.040

0.005~0.067

0.0240.023

N.D.C ~0.069

0.0190.027

Ni

N.D.~0.087

0.0160.018

N.D.~0.087

0.0190.020

0.002~0.029

0.0090.010

0.003~0.040

0.0140.013

N.D.~0.039

0.0110.014

0.005~0.039

0.0210.013

0.003~0.029

0.0120.010

0.010~0.039

0.0210.012

N.D.~0.020

0.0090.007

N.D.~0.084

0.0280.039

0.001~0.031

0.0160.011

N.D. ~0.026

0.0100.010

Pb

Amount (mg/g)
Sn

N.D.~0.330

0.0190.038

N.D.~0.093

0.0130.018

N.D.~0.330

0.0630.119

N.D.~0.021

0.0060.008

N.D. ~0.028

0.0140.012

N.D.~0.031

0.0120.012

N.D.~0.015

0.0070.007

N.D.~0.115

0.0220.042

N.D.~0.103

0.0200.037

N.D.~0.041

0.0150.016

N.D.~0.036

0.0140.014

0.007~0.084

0.0360.026

()

1.097~6.366

2.9090.992

1.097~6.366

2.6161.088

1.862~3.168

2.4260.452

2.389~4.788

3.0380.816

2.047~3.947

2.8780.732

2.737~4.983

3.331.0.760

2.884~4.875

3.5970.708

1.458~2.477

2.0310.424

2.006~3.354

2.5270.421

3.542~6.109

4.7480.790

2.389~3.970

3.0850.562

2.191~3.167

2.688.0.371

Zn

0.001~1.515

0.1880.305

0.088~0.568

0.0880.127

0.011~0.217

0.1000.067

0.010~0.049

0.0280.012

0.366~1.132

0.6440.295

0.117~0.630

0.3330.189

0.212~1.515

0.8850.492

0.001~0.026

0.0070.009

0.004~0.020

0.0100.007

0.020~0.060

0.0330.016

0.033~0.121

0.0590.032

0.037~0.577

0.1670.187

Hg

Ann. Rept. BFDA

0.330
g/g
7.
4 . 7 4 8 g / g
(3.542 ~ 6.109 g/g)
2.031 g/g (1.458 ~ 2.477 g/g)

6.366 mg/g
8.
()0.885 g/g
(0.212 ~ 1.515 g/g)
0.007 g/g (0.001 ~ 0.026 g/g)
()
1.515 g/g
100
1.000 g/g

1.369 g/g (0.640 ~


1.954 g/g)
1.000 g/g1.097 ~ 6.366 g/g

~ 1.954 g/g)
0.100 g/g (N.D. ~ 0.208 g/g)

1.954 g/g
4.
0.041 g/g (0.014
~ 0.079 g/g)
0.011 g/g (N.D. ~ 0.046 g/g)

0.112 g/g
5.
0 . 0 2 8 g / g
(N.D. ~ 0.084 g/g)
0.009 g/g (0.002 ~ 0.029 g/g)

0.087 mg/g
6.
0.063 g/g (N.D. ~
0.330 g/g)
0.007 g/g (N.D. ~ 0.021 g/g )

Cd

content (ug/g, wet weight)

0.1
0.08
0.06
0.04
0.02
0
hairtail

porgy

Pacific
saury

pomfret

parrotfish swordfish

tuna

-409-

shark

salmon

cod

others

Ann. Rept. BFDA

Cr

content (ug/g, wet weight)

0.1
0.08
0.06
0.04
0.02
0
hairtail

porgy

Pacific
saury

pomfret parrotfish swordfish

tuna

shark

salmon

cod

others

Cu

content (ug/g, wet weight)

2.5

1.5

0.5

0
hairtail

porgy

Pacific
saury

pomfret

parrotfish swordfish

tuna

shark

-410-

salmon

cod

others

Ni
0.12

content (ug/g, wet weight)

0.1
0.08
0.06
0.04
0.02
0
hairtail

porgy

Pacific
saury

pomfret

parrotfish swordfish

tuna

shark

salmon

cod

others

Pb

content (ug/g, wet weight)

0.1
0.08
0.06
0.04
0.02
0
hairtail

porgy

Pacific
saury

pomfret

parrotfish swordfish

tuna

-411-

shark

salmon

cod

others

Ann. Rept. BFDA

Sn
content (ug/g, wet weight)

0.35
0.3
0.25
0.2
0.15
0.1
0.05
0
hairtail

porgy

Pacific
saury

pomfret

parrotfish swordfish

tuna

shark

salmon

cod

others

Zn

content (ug/g, wet weight)

7
6
5
4
3
2
1
0
hairtail

porgy

Pacific
saury

pomfret parrotfish swordfish

tuna

shark

-412-

salmon

cod

others

Zn

content (ug/g, wet weight)

7
6
5
4
3
2
1
0
hairtail

porgy

Pacific
saury

pomfret parrotfish swordfish

tuna

shark

salmon

cod

others

Yaru (20)(normal waters)


(biological samples)
(Detection
limits)0.02 g/L0.004 g/g
0.2 g/L0.007 g g/g0.3 g/L
0.010 g/g0.02 g/g0.05 g/g
Tzen(21)
GFAAS
0.065 g/g
0.36 g/g0.98 g/g0.25 g/g

0.10.20.31.20.61.4
g/L
2 g/L
0.01 g/L

(())1.000
ppm1.0431.2571.5151.132
g/g

Tzen (21)
GFAAS
800
9001100
120020002100

7006501300
1500
120014002400
2300

-413-

-414-

35.9623.71
17.115.67
3.790.57
Huang, 2003
2.9090.992 In This Study
0.890.76

1.183.03

0.340.03
0.2700.353 0.0220.022

0.180.37
0.150.43
0.050.01
0.0160.018

0.0610.063 0.0200.021

0.040.05

0.010.02

0.050.01
0.0070.011 0.0110.012

U.S.A.

rivers & the Great


lake
bottom feeder sh
predator sh
Taiwan
eastern coast
Taiwan, R.O.C markets

0.0050.007
Gulf coast
Saudi Arabia

3.310.39

0.170.06
0.110.02
western coast

0.820.10
0.150.02
0.420.10

Egypt
United Arab
Emirate

0.050.01

0.080.01

19.5510.78
1.030.49
0.940.76
1.280.42

1.290.71

38.2314.78
7.453.44
1.220.80
1.450.65
1.460.53

Zn (g/g)
Pb (g/g)
Ni (g/g)
Cu (g/g)
Cr (g/g)
Cd (g/g)

Sampling site
Iskenderun Bay
Mugil cephalus
Trachurus
mediterraneus
six Governorates
Country
Turkey

Reference
Yilmaz, 2003

0.0010.0040.0030.0060.005
0.01 g/g0.01 g/g0.0005
g/g

Huang(22)2002311
20

0.050.010.34
0.030.050.013.790.57 g/g(
)100

0.0070.0110.270
0.0220.0160.0192.909 0.188
g/g()

100
(0.007 g/g)(0.011
g/g)(0.016 g/g)
1995Gomaa (2)
(0.050 g/g)(0.08 g/g)(0.15
g/g)(2.909 g/g)
2000Al-Yousuf (23)
3.31 g/g
2002Al-Salen and Shinwari(24)
(0.005 g/g)(0.020 g/g)

(25)

1.369 g/g
(0.640 ~ 1.954 g/g)
2000Al-Yousuf (24)
Arabian GulfLethrinus
lentjan1995

Gomaa et al., 1995


Al-Yousuf et al.,
2000
Al-Saleh and
Shinwari, 2002
Kidwell et al., 1995

Ann. Rept. BFDA

Kidwell (26)

568%
2.516 g/g
Tzen (21) 2003
Alosa caspia
(2.902.93 g/g)2003
Yilmaz(27)Iskenderun Bay

()

0.0190.038 g/g1998
Takahashi (28)Suruga

0.007 ~ 0.063 g/g


Nakagawa (29)
199734()
1.15 ~ 3.01 g/g
()(0.212 ~
1.515 g/g)Storelli(30)

0.17 ~ 10.51 g/g


(0.366 ~ 1.132 g/g)

(5)

()

(Maximum
allowed/recommend levels)(The
Australian Food Standards Code)
()
(Barramundi)(ling)

(mg/kg)

0.2

0.1

0.007 (N.D.~0.067)

1.0

0.011 (N.D.~0.082)

100

30

0.270 (N.D.~1.954)

1.5

0.5

0.016 (N.D.~0.087)

50 mg/kg

2.909 mg/g
(1.097~6.366)

:2002(5)

(orange roughy)(rays)
1.0 mg/
kg
0.5 mg/kg(Guideline/Tolerances
of various Chemical Contaminants in
Canada)(()
)
0.5 ppm

0.2 ppm(Food Sanitation Law)


0.4 ppm
0.3 ppm(European Community)
(angelfish)

-415-

Ann. Rept. BFDA

(35)

(Flounder)(Cod)(Catfish)
(Trout)(Pollock)(Clams)
(Shrimp)(Scallops)(Lobster)

()(tilefish)(king
mackerel)()
FDA
12(ounces)
(36)()

(Tolerable Intake level)(The


Australian Food Standards Code)
(Tolerable Weekly
Intake)2.8 g Hg/kg body weight
(Guideline/Tolerances of various Chemical
Contaminants in Canada)
(Provisional Tolerable
Daily Intake)0.47 g Hg/kg body weight
0.2 g Hg/kg body
weightFAO/WHO
(Joint FAO/WHO Expert Committee on Food
Additives, JECFA)
(provisional tolerable weekly
Intake, PTWI)3.3 g/kg body weight(35)
60

(atalantic catfish)(bass)
(blueling)(bonito)(eel)
(halibut)(little tuna)
(marlin)(pike)(plain bonito)
(portuguese)(dogfish)
(redfish)(sail fish)
(scabbard fish)
(shark)(snake mackerel)
(sturgeon)()
1 mg /kg
0.5 mg/kg(European Statutory
Standard)0.3 mg Hg/kg
(action
level)1.0 ppm(local
trigger level)0.5 ppmWHO/FAO
(predators)
0.5 ppm
()
1.0 ppm(31)

100
1.0
ppm
100()
(1.043 1.257
1.5151.132 g/g)
(European Communities)
1.0 ppm (Commission Regulation
EC no. 466/2001)(32)The United States
Environmental Protection Agency (EPA)(33)
90 ~ 100%
1.00 g/g

2.0 ppm
(34)

-416-

materials) 5 mL
10 mL

100

107
300.007
g/g (N.D. ~ 0.067 g/g)
0.011 g/g (N.D. ~ 0.082 g/g)
0.270 g/g (N.D. ~ 1.954 g/g)
0.022 g/g (N.D. ~ 0.112 g/g)
0.016 g/g (N.D. ~ 0.087 g/g)
0.019 g/g (N.D. ~ 0.330
g/g)2.909 g/g (1.097
~ 6.366 g/g)0.188 g/g
(0.001 ~ 1.515 g/g)100
1.0 g/g
1.0 g/g
()

198 mg
10011
0.188 mg/g
1053

()

Storelli
Marcotrigiano(37)()

0.950.92()
30 ~ 90
(0.47 ~ 0.67 g/g, wet
weight)1.0 mg/g
10030 ~ 90
(0.82 ~ 1.57 g/
g)
()

1. 1988
437-50
2. M. N. E. Gomaa, A. A. K. Abou-Arab, A.
Badawy, and N. Khayria. 1995. Distribution
pattern of some heavy metals in Egyptian sh
organs. Food Chemistry, 53:385-389.
3. 2000
(I)

4. 1989

(Cd)(Cr)
(Cu)(Ni)(Pb)(Sn)(Zn)

(r)0.999
(certified reference

-417-

Ann. Rept. BFDA

pp.116 ~ 130.
5. 2002

pp.1 ~ 116
6. 2000
pp.194 ~ 206
7. F. H . N i e l s e n . 1 9 8 8 . P o s s i b l e f u t u r e
implications of ultratrace elements in human
health and disease. pp. 277-293. In A. R. Liss
(ed.) Essential and toxic trace elements in
human health and disease. Current Topics in
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Total mercury levels in muscle tissue of
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Analysis and Investigation of Heavy Metals in Marine


Fishes by GFAAS/FLAAS/Hg-AFS in Taiwan
RU-CHIA SHIH, SYR-SONG CHEN, MEI-HUA CHANG, YA-CHI CHIU, YI-RU
CHEN, CHIEU-CHEN CHENG AND SHIN-SHOU CHOU
Food Chemistry Division

Abstract
In order to analyze heavy metals in sh samples, a simple and rapid wet digestion method was developed
for complete destruction of the marine sh tissue samples, as opposed to the conventional dry-ashing procedures.
An atomic absorption spectrometer equipped with Zeeman background correction was used for the determination
of heavy metals of Cd, Cr, Cu, Ni, Pb, and Sn. Zn was analyzed by a ame atomic absorption spectrometer. Hg
was determined by a mercury atomic uorescence spectrometer after the microwave digestion pretreatment. The
method was evaluated using certified reference materials. The developed method was applied to analyze 100
marine sh samples, including hairtail, porgy, Pacic saury, pomfret, parrotsh, swordsh, tuna, shark, salmon,
cod, and other specimens. The results showed that average content of Cd, Cr, Cu, Ni, Pb, Sn, Zn, and Hg was
0.007 mg/g (N.D.~0.067 mg/g), 0.011 mg/g (N.D.~0.082 mg/g), 0.270 mg/g (N.D.~1.954 mg/g), 0.022 mg/g
(N.D.~0.112 mg/g), 0.016 mg/g (N.D~0.087 mg/g), 0.019 mg/g (N.D.~0.330 mg/g), 2.909 mg/g (1.097~6.366
mg/g), and 0.188 mg/g (0.001~1.515 mg/g) , respectively.

Key words: heavy metals, graphite furnace atomic absorption spectrophotometer (GFAAS),
flame atomic absor ption spectrophotometer (FLAAS), mercur y atomic
uorescence spectrometer (Hg-AFS), sh

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