aoac会议课件-食品中多种砷形态

重金属污染Heavy

metal

pollution污染来源Pollution

sources危害特性Damage

Performance蓄积性Accumulation；慢性作用Chronic

effect；不可逆的损害Irreversible

damage

；不易察觉，容易忽视Apt

to

overlook；7重金属污染主要食品种类The

main

types

of

heavy

metal

contamination

of

food砷污染的问题不容忽视Arsenic

pollution

problems

can

not

be

ignored食品中砷的主要来源The

main

sources

of

arsenic

in

food砷的毒性与危害Toxicity

and

harm

of

arsenic各国

和国际组织对砷的形态分析给予很大关注anizations

givenysis

of

Arsenicernments

and

internationalgreat

attention

to

speciation欧盟文件EPA（

环境保护局）了四种毒性较高的砷的形态分析的方法As(III)

-

As(V)

–MMA

–DMAIAEA（国际原子能机构）Development

and

validation

ofspeciation ysis

-

ProjectHighly

toxicLess

toxicSpeciesH3AsAsIIIAsVMMAVDMAVAsCAsBAsSLD5031420700-1800700-26006500>10000>8000Non-toxic砷的形态与毒性Species

and

toxicity

of

arsenicLD50

in

rats

(in

mg/kg):砷的形态Arsenic

Species元素形态与其毒性密切相关Speciation

and

toxicity

of

closely

related;古代炼丹就是炼的砷和

；紫菜中有较高的砷含量，砷的循环Arsenic

in

the

circulation元素测定和形态分析Element

determination

and

speciation

ysis测定总量已不能满足食品安全分析评价的需要ysis

andDetermination

oftotal

has

been

unable

to

meet

the

needsassessment

of

food

safety

；As、Hg、Se、Sn;现代分析技术为元素形态分析提供了技术保障；Modernspeciationysis

technology

provides

technical

guarantee

for

elementalysis；从总量分析向形态分析发展From

the

total

ysis

to

the

development

of

speciation ysis

；砷形态分析的方法Methods

for

arsenic

speciationysis分离部分Separation

part气相色谱（GC）冷阱分离（CT）液相色谱（LC）毛细管电泳（CE）检测部分Detection

part原子吸收（AAS）原子荧光（AFS）原子发射（ICP-OES）等离子质谱（ICP-MS）接口部分ConnectionpartMethod

of

LC-HGAFS食品样品高速离心0.45µm

滤膜进样(100

µL)分离固体颗粒除固体颗粒HPLC-HG-AFS样品分析甲醇/水超声提取提取目标化合物砷形态分析的方法Methods

for

arsenic

speciationysis标准色谱图The

standard

chromatogram紫菜中As形态The

arsenic

species

in

laver紫菜的加标回收The

recovery

of

standard

addition

in

laverMethod

of

HPLC-ICP-MS不同浓度流动相对应砷形态的谱图Different

concentrations

of

flow

corresponding

spectra

ofarsenicA

5:95,B

10:90,C

15:851

ASA，2

NIT，3

ROXThe

standard

chromatogram

(0.1-2ug/mL)HPLC-ICP-MS

chromatogram1

.

0

02

.

0

03

.

0

07

.

0

08

.

0

09

.

0

06

0

0

5

5

0

5

0

0

4

5

0

4

0

0

3

5

0

3

0

0

2

5

0

2

0

0

1

5

0

1

0

0

5

0

0T

i

m

e

-

-

>A

b

u

n

d

a

n

c

eT

I

C

:

S

7

.

D

(

+

,

-

)1

.

5

31

.

0

02

.

0

03

.

0

04

.

0

05

.

0

06

.

0

07

.

0

08

.

0

09

.

0

03

5

0

3

0

0

2

5

0

2

0

0

05

0

0

4

5

0

6

0

0

5

5

0

T

i

m

e

-

->4

.

0

0

A

b

u

n

d

a

n

c

e

6

.

0

0T

I

C

:

S

5

.

D

(

+

,

-

)1

.

5

32

.

0

25

.

1

27

.

5

1Simultaneous

differmination

As

and

Se一、高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS)反相离子对色谱分离流动相浓度流动相酸度离子对试剂浓度Simultaneous

differmination

As

and

Se形态蘑菇鱼肉本底值（mg/Kg）加标量（mg/Kg）平均回收率（%）本底值（mg/Kg）加标量（mg/Kg）平均回收率（%）AsIIIND0.2100.2ND0.2101.5DMAND0.298.6ND0.293.9MMAND0.291.5ND0.296.4AsV0.1040.2101.80.2850.2102.2SeIV0.1210.299.80.010.2100.5SeCys0.1060.289.40.4860.295.2SeMet0.0631.086.9ND1.089.7实际样品检测和加标回收实验结果The

actual

specimen

detection

and

recovery

experimentsSimultaneous

differmination

As

and

Se二、液相色谱-原子荧光光谱法(LC-HG-AFS)205.5677.56.5pH保留时间/minS

e

C

y

sS

e

(

I

V

)S

e

M

e

t765432105.566.5pH77.5保留时间/minAs(III)DMAMMAAs(V)876543210105020

30

40流动相浓度/mM保留时间/minSeCysSe(IV)SeMet105020

30

40流动相浓度/mM保留时间/minA

s

(

I

I

I)DMAMMAAs(V)As、Se同时测定20701201702202705101520HCl

/%

(v/v)信噪比SeCysSe(IV)SeMetAs(III)DMAMMAAs(V)02040608010012014011.11.21.31.51.61.71.81.4KBH4/%(w/v)信噪比SeCysSe(IV)SeMetAs(III)DMAMMAAs(V)020406080100120140160300350400500550600450载气/mL/min信噪比SeCysSe(IV)SeMetAs(III)DMAMMAAs(V)0204060801001201401605006009001000700800气流量/mL/min信噪比SeCysSe(IV)SeMetAs(III)DMAMMAAs(V)Simultaneous

differmination

As

and

Se提取剂SeCysSe(IV)SeMetAs(III)DMAMMAAs(V)H2O,(20℃)样品中含量－a108.1————0.284加标回收率92.1110.193.396.6102.6111.2107.8H2O,(100℃)样品中含量—107.3————0.265加标回收率(%)91.2114.7101.294.497.698.4108.0主要问题—前处理Main

problem--Pretreatment1、提取效率；Extraction

efficiency；2、形态转化；Species

transition；3、不同提取方法的可比性；The

comparability

of

different

extraction

methods

；主要问题—方法验证Main

problem--Method

Verification1、添加回收试验；Add

recovery

test2、标准品和参考物质；Standard

and

reference

material3、测定方法的差异；Method

of

difference主要问题—硬件和Main

problem-

Hardware

and

software1、联用标准接口；Combined

with

the

standard

interface2、色谱柱的选择；The

selection

of

chromatography

column3、元素形态分析仪Element

speciation；yzer