食品安全质量检测学报

组成	时间/min
流动相A/%	58	78	90	90	58	58
流动相B/%	42	22	10	10	42	42

组成

时间/min

0.00

22.00

25.00

32.00

32.01

37.00

流动相A/%

流动相B/%

组成	时间/min
流动相A/%	58	78	90	90	58	58
流动相B/%	42	22	10	10	42	42

组成

时间/min

0.00

22.00

25.00

32.00

32.01

37.00

流动相A/%

流动相B/%

化合物	保留时间/min	线性方程	r²	检出限/(mg/kg)	定量限/(mg/kg)
色胺	13.3	Y=2.1263X-1.0603	0.9992	0.93	3.10
β-苯乙胺	15.6	Y=2.1228X-2.2119	0.9993	1.05	3.51
腐胺	17.0	Y=4.2678X-2.2157	0.9998	0.32	1.08
尸胺	18.5	Y=3.7806X-2.5078	0.9995	0.38	1.28
组胺	19.7	Y=2.1383X+1.5954	0.9999	0.69	2.31
章鱼胺	20.9	Y=2.1103X+1.4512	0.9991	1.22	4.06
酪胺	26.6	Y=2.2038X+1.9809	0.9995	0.97	3.25
亚精胺	28.0	Y=2.1319X+1.8553	0.9995	0.96	3.19
精氨	33.0	Y=2.0865X+1.5730	0.9992	2.28	7.59

化合物

保留时间/min

线性方程

r²

检出限/(mg/kg)

定量限/(mg/kg)

色胺

13.3

Y=2.1263X-1.0603

0.9992

0.93

3.10

β-苯乙胺

15.6

Y=2.1228X-2.2119

0.9993

1.05

3.51

腐胺

17.0

Y=4.2678X-2.2157

0.9998

0.32

1.08

尸胺

18.5

Y=3.7806X-2.5078

0.9995

0.38

1.28

组胺

19.7

Y=2.1383X+1.5954

0.9999

0.69

2.31

章鱼胺

20.9

Y=2.1103X+1.4512

0.9991

1.22

4.06

酪胺

26.6

Y=2.2038X+1.9809

0.9995

0.97

3.25

亚精胺

28.0

Y=2.1319X+1.8553

0.9995

0.96

3.19

精氨

33.0

Y=2.0865X+1.5730

0.9992

2.28

7.59

化合物	保留时间/min	线性方程	r²	检出限/(mg/kg)	定量限/(mg/kg)
色胺	13.3	Y=2.1263X-1.0603	0.9992	0.93	3.10
β-苯乙胺	15.6	Y=2.1228X-2.2119	0.9993	1.05	3.51
腐胺	17.0	Y=4.2678X-2.2157	0.9998	0.32	1.08
尸胺	18.5	Y=3.7806X-2.5078	0.9995	0.38	1.28
组胺	19.7	Y=2.1383X+1.5954	0.9999	0.69	2.31
章鱼胺	20.9	Y=2.1103X+1.4512	0.9991	1.22	4.06
酪胺	26.6	Y=2.2038X+1.9809	0.9995	0.97	3.25
亚精胺	28.0	Y=2.1319X+1.8553	0.9995	0.96	3.19
精氨	33.0	Y=2.0865X+1.5730	0.9992	2.28	7.59

化合物

保留时间/min

线性方程

r²

检出限/(mg/kg)

定量限/(mg/kg)

色胺

13.3

Y=2.1263X-1.0603

0.9992

0.93

3.10

β-苯乙胺

15.6

Y=2.1228X-2.2119

0.9993

1.05

3.51

腐胺

17.0

Y=4.2678X-2.2157

0.9998

0.32

1.08

尸胺

18.5

Y=3.7806X-2.5078

0.9995

0.38

1.28

组胺

19.7

Y=2.1383X+1.5954

0.9999

0.69

2.31

章鱼胺

20.9

Y=2.1103X+1.4512

0.9991

1.22

4.06

酪胺

26.6

Y=2.2038X+1.9809

0.9995

0.97

3.25

亚精胺

28.0

Y=2.1319X+1.8553

0.9995

0.96

3.19

精氨

33.0

Y=2.0865X+1.5730

0.9992

2.28

7.59

化合物	1倍定量限	2倍定量限	5倍定量限
色胺	89.6~103.5	2.8~4.6	87.8~104.6	2.3~4.4	88.6~105.8	2.9~4.0
β-苯乙胺	86.5~105.4	2.6~4.5	87.8~102.1	2.6~4.9	90.9~103.6	2.2~4.7
腐胺	87.5~104.6	1.5~3.6	86.3~105.7	2.1~4.7	88.1~104.3	2.5~4.9
尸胺	85.2~104.3	1.9~4.7	86.9~105.1	1.9~4.0	89.6~106.5	1.8~4.5
组胺	90.1~102.3	2.7~4.9	87.9~102.6	2.4~4.6	89.5~102.4	2.0~4.8
章鱼胺	92.1~105.2	1.8~4.5	92.7~106.7	1.9~4.8	91.1~105.1	2.2~4.6
酪胺	90.8~103.5	2.1~4.6	91.2~103.2	3.2~4.9	92.2~103.4	3.1~4.8
亚精胺	86.5~102.1	1.9~4.0	85.6~103.5	2.0~4.8	86.9~102.5	1.7~4.6
精胺	92.1~103.5	2.5~4.8	91.2~104.5	2.2~4.6	93.0~104.3	2.4~4.9

化合物

1倍定量限

2倍定量限

5倍定量限

加标回收率

RSDs

加标回收率

RSDs

加标回收率

RSDs

色胺

89.6~103.5

2.8~4.6

87.8~104.6

2.3~4.4

88.6~105.8

2.9~4.0

β-苯乙胺

86.5~105.4

2.6~4.5

87.8~102.1

2.6~4.9

90.9~103.6

2.2~4.7

腐胺

87.5~104.6

1.5~3.6

86.3~105.7

2.1~4.7

88.1~104.3

2.5~4.9

尸胺

85.2~104.3

1.9~4.7

86.9~105.1

1.9~4.0

89.6~106.5

1.8~4.5

组胺

90.1~102.3

2.7~4.9

87.9~102.6

2.4~4.6

89.5~102.4

2.0~4.8

章鱼胺

92.1~105.2

1.8~4.5

92.7~106.7

1.9~4.8

91.1~105.1

2.2~4.6

酪胺

90.8~103.5

2.1~4.6

91.2~103.2

3.2~4.9

92.2~103.4

3.1~4.8

亚精胺

86.5~102.1

1.9~4.0

85.6~103.5

2.0~4.8

86.9~102.5

1.7~4.6

精胺

92.1~103.5

2.5~4.8

91.2~104.5

2.2~4.6

93.0~104.3

2.4~4.9

化合物	1倍定量限	2倍定量限	5倍定量限
色胺	89.6~103.5	2.8~4.6	87.8~104.6	2.3~4.4	88.6~105.8	2.9~4.0
β-苯乙胺	86.5~105.4	2.6~4.5	87.8~102.1	2.6~4.9	90.9~103.6	2.2~4.7
腐胺	87.5~104.6	1.5~3.6	86.3~105.7	2.1~4.7	88.1~104.3	2.5~4.9
尸胺	85.2~104.3	1.9~4.7	86.9~105.1	1.9~4.0	89.6~106.5	1.8~4.5
组胺	90.1~102.3	2.7~4.9	87.9~102.6	2.4~4.6	89.5~102.4	2.0~4.8
章鱼胺	92.1~105.2	1.8~4.5	92.7~106.7	1.9~4.8	91.1~105.1	2.2~4.6
酪胺	90.8~103.5	2.1~4.6	91.2~103.2	3.2~4.9	92.2~103.4	3.1~4.8
亚精胺	86.5~102.1	1.9~4.0	85.6~103.5	2.0~4.8	86.9~102.5	1.7~4.6
精胺	92.1~103.5	2.5~4.8	91.2~104.5	2.2~4.6	93.0~104.3	2.4~4.9

化合物

1倍定量限

2倍定量限

5倍定量限

加标回收率

RSDs

加标回收率

RSDs

加标回收率

RSDs

色胺

89.6~103.5

2.8~4.6

87.8~104.6

2.3~4.4

88.6~105.8

2.9~4.0

β-苯乙胺

86.5~105.4

2.6~4.5

87.8~102.1

2.6~4.9

90.9~103.6

2.2~4.7

腐胺

87.5~104.6

1.5~3.6

86.3~105.7

2.1~4.7

88.1~104.3

2.5~4.9

尸胺

85.2~104.3

1.9~4.7

86.9~105.1

1.9~4.0

89.6~106.5

1.8~4.5

组胺

90.1~102.3

2.7~4.9

87.9~102.6

2.4~4.6

89.5~102.4

2.0~4.8

章鱼胺

92.1~105.2

1.8~4.5

92.7~106.7

1.9~4.8

91.1~105.1

2.2~4.6

酪胺

90.8~103.5

2.1~4.6

91.2~103.2

3.2~4.9

92.2~103.4

3.1~4.8

亚精胺

86.5~102.1

1.9~4.0

85.6~103.5

2.0~4.8

86.9~102.5

1.7~4.6

精胺

92.1~103.5

2.5~4.8

91.2~104.5

2.2~4.6

93.0~104.3

2.4~4.9

化合物	GB 5009.208—2016	本研究方法
色胺	82.3~101.3	7.9~9.8	94.6~103.6	2.3~3.1
β-苯乙胺	85.2~102.1	7.4~9.5	94.0~104.2	2.0~3.2
腐胺	81.6~101.0	8.0~9.7	93.9~102.9	1.9~3.8
尸胺	82.9~103.2	7.7~9.6	93.0~104.6	1.9~3.3
组胺	86.5~102.7	7.6~9.4	95.6~103.9	2.5~3.6
章鱼胺	82.5~103.8	7.5~9.6	93.6~103.4	2.3~3.8
酪胺	83.5~102.4	7.4~9.3	94.2~104.7	2.0~3.5
亚精胺	82.4~103.1	7.6~9.7	94.1~104.1	2.3~3.7
精胺	83.4~102.8	8.2~9.8	94.8~103.9	2.4~3.7

化合物

GB 5009.208—2016

本研究方法

加标回收率

RSDs

加标回收率

RSDs

色胺

82.3~101.3

7.9~9.8

94.6~103.6

2.3~3.1

β-苯乙胺

85.2~102.1

7.4~9.5

94.0~104.2

2.0~3.2

腐胺

81.6~101.0

8.0~9.7

93.9~102.9

1.9~3.8

尸胺

82.9~103.2

7.7~9.6

93.0~104.6

1.9~3.3

组胺

86.5~102.7

7.6~9.4

95.6~103.9

2.5~3.6

章鱼胺

82.5~103.8

7.5~9.6

93.6~103.4

2.3~3.8

酪胺

83.5~102.4

7.4~9.3

94.2~104.7

2.0~3.5

亚精胺

82.4~103.1

7.6~9.7

94.1~104.1

2.3~3.7

精胺

83.4~102.8

8.2~9.8

94.8~103.9

2.4~3.7

化合物	GB 5009.208—2016	本研究方法
色胺	82.3~101.3	7.9~9.8	94.6~103.6	2.3~3.1
β-苯乙胺	85.2~102.1	7.4~9.5	94.0~104.2	2.0~3.2
腐胺	81.6~101.0	8.0~9.7	93.9~102.9	1.9~3.8
尸胺	82.9~103.2	7.7~9.6	93.0~104.6	1.9~3.3
组胺	86.5~102.7	7.6~9.4	95.6~103.9	2.5~3.6
章鱼胺	82.5~103.8	7.5~9.6	93.6~103.4	2.3~3.8
酪胺	83.5~102.4	7.4~9.3	94.2~104.7	2.0~3.5
亚精胺	82.4~103.1	7.6~9.7	94.1~104.1	2.3~3.7
精胺	83.4~102.8	8.2~9.8	94.8~103.9	2.4~3.7

化合物

GB 5009.208—2016

本研究方法

加标回收率

RSDs

加标回收率

RSDs

色胺

82.3~101.3

7.9~9.8

94.6~103.6

2.3~3.1

β-苯乙胺

85.2~102.1

7.4~9.5

94.0~104.2

2.0~3.2

腐胺

81.6~101.0

8.0~9.7

93.9~102.9

1.9~3.8

尸胺

82.9~103.2

7.7~9.6

93.0~104.6

1.9~3.3

组胺

86.5~102.7

7.6~9.4

95.6~103.9

2.5~3.6

章鱼胺

82.5~103.8

7.5~9.6

93.6~103.4

2.3~3.8

酪胺

83.5~102.4

7.4~9.3

94.2~104.7

2.0~3.5

亚精胺

82.4~103.1

7.6~9.7

94.1~104.1

2.3~3.7

精胺

83.4~102.8

8.2~9.8

94.8~103.9

2.4~3.7

样品名称	色胺	β-苯乙胺	腐胺	尸胺	组胺	章鱼胺	酪胺	亚精胺	精胺
马鲛鱼1	N.D.	N.D.	N.D.	32.2	N.D.	N.D.	10.0	N.D.	N.D.
马鲛鱼2	N.D.	N.D.	N.D.	24.9	N.D.	N.D.	N.D.	N.D.	N.D.
马鲛鱼3	N.D.	N.D.	26.2	N.D.	N.D.	N.D.	15.2	N.D.	N.D.
马鲛鱼4	N.D.	N.D.	N.D.	13.1	N.D.	N.D.	N.D.	N.D.	N.D.
马鲛鱼5	N.D.	N.D.	N.D.	15.1	N.D.	N.D.	N.D.	N.D.	N.D.
马鲛鱼6	N.D.	N.D.	N.D.	15.0	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼1	N.D.	34.1	N.D.	19.7	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼2	N.D.	26.7	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼3	N.D.	25.1	N.D.	18.0	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼4	N.D.	30.3	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼5	N.D.	25.8	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼6	N.D.	26.1	16.0	18.1	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼7	N.D.	28.6	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼8	N.D.	26.2	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼9	N.D.	27.8	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼10	N.D.	27.1	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼11	N.D.	N.D.	N.D.	13.2	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼12	N.D.	27.3	N.D.	13.7	N.D.	N.D.	N.D.	N.D.	N.D.
秋刀鱼1	N.D.	24.0	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼1	N.D.	N.D.	N.D.	20.2	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼2	N.D.	N.D.	N.D.	14.8	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼3	N.D.	N.D.	N.D.	15.7	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼4	N.D.	28.2	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼5	N.D.	29.2	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼6	N.D.	29.6	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.

样品名称

色胺

β-苯乙胺

腐胺

尸胺

组胺

章鱼胺

酪胺

亚精胺

精胺

马鲛鱼1

N.D.

32.2

N.D.

10.0

N.D.

马鲛鱼2

N.D.

24.9

N.D.

马鲛鱼3

N.D.

26.2

N.D.

15.2

N.D.

马鲛鱼4

N.D.

13.1

N.D.

马鲛鱼5

N.D.

15.1

N.D.

马鲛鱼6

N.D.

15.0

N.D.

青占鱼1

N.D.

34.1

N.D.

19.7

N.D.

青占鱼2

N.D.

26.7

N.D.

青占鱼3

N.D.

25.1

N.D.

18.0

N.D.

青占鱼4

N.D.

30.3

N.D.

青占鱼5

N.D.

25.8

N.D.

青占鱼6

N.D.

26.1

16.0

18.1

N.D.

青占鱼7

N.D.

28.6

N.D.

青占鱼8

N.D.

26.2

N.D.

青占鱼9

N.D.

27.8

N.D.

青占鱼10

N.D.

27.1

N.D.

青占鱼11

N.D.

13.2

N.D.

青占鱼12

N.D.

27.3

N.D.

13.7

N.D.

秋刀鱼1

N.D.

24.0

N.D.

竹荚鱼1

N.D.

20.2

N.D.

竹荚鱼2

N.D.

14.8

N.D.

竹荚鱼3

N.D.

15.7

N.D.

竹荚鱼4

N.D.

28.2

N.D.

竹荚鱼5

N.D.

29.2

N.D.

竹荚鱼6

N.D.

29.6

N.D.

样品名称	色胺	β-苯乙胺	腐胺	尸胺	组胺	章鱼胺	酪胺	亚精胺	精胺
马鲛鱼1	N.D.	N.D.	N.D.	32.2	N.D.	N.D.	10.0	N.D.	N.D.
马鲛鱼2	N.D.	N.D.	N.D.	24.9	N.D.	N.D.	N.D.	N.D.	N.D.
马鲛鱼3	N.D.	N.D.	26.2	N.D.	N.D.	N.D.	15.2	N.D.	N.D.
马鲛鱼4	N.D.	N.D.	N.D.	13.1	N.D.	N.D.	N.D.	N.D.	N.D.
马鲛鱼5	N.D.	N.D.	N.D.	15.1	N.D.	N.D.	N.D.	N.D.	N.D.
马鲛鱼6	N.D.	N.D.	N.D.	15.0	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼1	N.D.	34.1	N.D.	19.7	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼2	N.D.	26.7	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼3	N.D.	25.1	N.D.	18.0	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼4	N.D.	30.3	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼5	N.D.	25.8	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼6	N.D.	26.1	16.0	18.1	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼7	N.D.	28.6	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼8	N.D.	26.2	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼9	N.D.	27.8	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼10	N.D.	27.1	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼11	N.D.	N.D.	N.D.	13.2	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼12	N.D.	27.3	N.D.	13.7	N.D.	N.D.	N.D.	N.D.	N.D.
秋刀鱼1	N.D.	24.0	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼1	N.D.	N.D.	N.D.	20.2	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼2	N.D.	N.D.	N.D.	14.8	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼3	N.D.	N.D.	N.D.	15.7	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼4	N.D.	28.2	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼5	N.D.	29.2	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼6	N.D.	29.6	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.

样品名称

色胺

β-苯乙胺

腐胺

尸胺

组胺

章鱼胺

酪胺

亚精胺

精胺

马鲛鱼1

N.D.

32.2

N.D.

10.0

N.D.

马鲛鱼2

N.D.

24.9

N.D.

马鲛鱼3

N.D.

26.2

N.D.

15.2

N.D.

马鲛鱼4

N.D.

13.1

N.D.

马鲛鱼5

N.D.

15.1

N.D.

马鲛鱼6

N.D.

15.0

N.D.

青占鱼1

N.D.

34.1

N.D.

19.7

N.D.

青占鱼2

N.D.

26.7

N.D.

青占鱼3

N.D.

25.1

N.D.

18.0

N.D.

青占鱼4

N.D.

30.3

N.D.

青占鱼5

N.D.

25.8

N.D.

青占鱼6

N.D.

26.1

16.0

18.1

N.D.

青占鱼7

N.D.

28.6

N.D.

青占鱼8

N.D.

26.2

N.D.

青占鱼9

N.D.

27.8

N.D.

青占鱼10

N.D.

27.1

N.D.

青占鱼11

N.D.

13.2

N.D.

青占鱼12

N.D.

27.3

N.D.

13.7

N.D.

秋刀鱼1

N.D.

24.0

N.D.

竹荚鱼1

N.D.

20.2

N.D.

竹荚鱼2

N.D.

14.8

N.D.

竹荚鱼3

N.D.

15.7

N.D.

竹荚鱼4

N.D.

28.2

N.D.

竹荚鱼5

N.D.

29.2

N.D.

竹荚鱼6

N.D.

29.6

N.D.

丹磺酰氯柱前衍生-反相高效液相色谱法同时测定水产品中9种生物胺

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周朗君 ¹^,² , 陈钦 ¹^,² , 李秀英 ¹^,²^,^*

食品安全质量检测学报 | 本期重点：广州检验检测认证集团有限公司 2025,16(5): 24-31

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食品安全质量检测学报 | 本期重点：广州检验检测认证集团有限公司 2025, 16(5): 24-31

丹磺酰氯柱前衍生-反相高效液相色谱法同时测定水产品中9种生物胺

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周朗君¹^,², 陈钦¹^,², 李秀英¹^,²^,^*

作者信息

1.广州检验检测认证集团有限公司, 广州 511447

2.国家加工食品质量检验检测中心(广东), 广州 511447

周朗君(1991—), 女, 硕士, 高级工程师, 主要研究方向为食品质量安全分析检测。E-mail: 1533846242@qq.com

通讯作者:

^* 李秀英(1984—), 女, 硕士, 高级工程师, 主要研究方向为食品质量安全分析检测。E-mail: 328444798@qq.com

Simultaneous determination of 9 kinds of biogenic amines in aquatic products by dansyl chloride precolumn derivatization-reverse phase high performance liquid chromatography

Lang-Jun ZHOU¹^,², Qin CHEN¹^,², Xiu-Ying LI¹^,²^,^*

Affiliations

1. Guangzhou Inspection Testing and Certification Group Co., Ltd., Guangzhou 511447, China

2. National Quality Testing Center for Processed Food (Guangdong), Guangzhou 511447, China

出版时间: 2025-03-15 doi: 10.19812/j.cnki.jfsq11-5956/ts.20241018004

文章导航

摘要

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目的建立丹磺酰氯柱前衍生-反相高效液相色谱法同时检测水产品中9种生物胺的检测方法。方法采用5%三氯乙酸水溶液提取, 10 mg/mL丹磺酰氯丙酮溶液衍生, 氨水终止衍生反应, 乙腈定容获得9种生物胺的丹磺酰氯衍生物待测溶液。试样溶液通过反相液相色谱检测, 以乙腈和水为流动相梯度洗脱, 采用C₁₈色谱柱分离, 紫外检测器在254 nm下检测。结果水产品中9种生物胺的定量限在1.08~7.59 mg/kg, 加标回收率在85.2%~106.7%, 精密度在1.5%~4.9%。采用所建立的方法测定广州市售的50批次高组胺鱼类, 结果发现, 广州市售的高组胺鱼类质量整体较好, β-苯乙胺和尸胺相对其他生物胺有较高检出率, 但含量均低于35 mg/kg, 色胺、组胺、章鱼胺、亚精胺、精氨均为未检出。结论该方法快速、简便、灵敏度高, 适用于水产品中9种生物胺的批量样品测定。

关键词

丹磺酰氯 / 柱前衍生 / 反相高效液相色谱法 / 水产品 / 生物胺

Abstract

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Objective To establish a detection method for simultaneously detecting 9 kinds of biogenic amines in aquatic products using the dansyl chloride precolumn derivazation-reverse phase high performance liquid chromatography. Methods The samples were extracted with a 5% trichloroacetic acid solution and derivatized with a 10 mg/mL dansyl chloride acetone solution. The derivatization reaction was terminated with ammonia, and the resulting solution containing the dansyl chloride derivatives of the 9 kinds of biogenic amines was made up to volume with acetonitrile. The sample solution was analyzed by reverse phase liquid chromatography using a C₁₈ column, with a mobile phase gradient of acetonitrile and water, and detected at 254 nm using a ultraviolet detector. Results The limits of quantitation of the 9 kinds of biogenic amines in aquatic products ranged from 1.08 to 7.59 mg/kg, with recovery rates ranging from 85.2% to 106.7% and precision ranging from 1.5% to 4.9%. The established method was used to analyze 50 batches of high-histamine fish sold in Guangzhou. The results revealed that the overall quality of the high-histamine fish in Guangzhou was good. β-phenylethylamine and cadaverine had relatively higher detection rates compared to other biogenic amines, but their content was all below 35 mg/kg. Histamine, putrescine, spermidine, agmatine, and arginine were not detected. Conclusion The method is fast, simple, and highly sensitive, making it suitable for batch sample determination of the 9 kinds of biogenic amines in aquatic products.

Key words

dansyl chloride / precolumn derivazation / reverse phase high performance liquid chromatography / aquatic product / biogenic amine

引用本文

周朗君, 陈钦, 李秀英. 丹磺酰氯柱前衍生-反相高效液相色谱法同时测定水产品中9种生物胺. 食品安全质量检测学报, 2025 , 16 (5) : 24 -31 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241018004

Lang-Jun ZHOU, Qin CHEN, Xiu-Ying LI. Simultaneous determination of 9 kinds of biogenic amines in aquatic products by dansyl chloride precolumn derivatization-reverse phase high performance liquid chromatography[J]. Journal of Food Safety & Quality, 2025 , 16 (5) : 24 -31 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241018004

正文

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0 引言

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生物胺, 是一组在生物体内扮演重要角色的含氨基有机化合物, 通常具有低分子量且呈碱性^[1-2], 包括但不限于色胺、β-苯乙胺、腐胺、尸胺、组胺、章鱼胺、酪胺、亚精胺和精胺等^[3]。生物胺广泛分布于多种食品中, 尤其是蛋白质含量较高的食品, 如各类水产品(包括鱼和虾的加工制品)、肉类、以及酒类(葡萄酒、啤酒、黄酒等)和调味品(醋和酱油)等^[4-5]。生物胺的生成机制为: 在食品的加工和储存过程中, 食品中的微生物产生的脱羧酶催化食品中的氨基酸发生脱羧反应生成了生物胺^[6-8]。虽然生物胺在人体生理调节中发挥着关键作用, 但一旦摄入过多的生物胺, 则会产生头晕、恶心、呕吐等过敏症状^[9-10], 因此, 欧盟^[11]、美国^[12]和中国都明确规定了食品中生物胺的限量值, 例如美国食品和药物管理局(food and drug administration, FDA)要求水产品中的组胺低于50 mg/kg, 欧盟要求不超过100 mg/kg, 我国GB 2733—2015《食品安全国家标准鲜、冻动物性水产品》规定高组胺鱼类组胺含量不得超过40 mg/100 g, 其他海水鱼类不超过20 mg/100 g, 我国的GB 7098—2015《食品安全国家标准罐头食品》鱼类罐头(仅适用于鲐鱼、鲹鱼、沙丁鱼)组胺限量标准为100 mg/100 g。

目前, 测定生物胺含量的主要方法有高效液相色谱法^[13-16]、高效液相色谱-串联质谱法^[17-20]、气相色谱法^[21-22]、气相色谱-串联质谱法^[23]、离子色谱法^[24-26]、分光光度法^[27-28]、薄层色谱法^[29-30]等。高效液相色谱-串联质谱法、气相色谱-串联质谱法的样品前处理无需衍生步骤, 分析时间短, 但设备较为昂贵, 运行维护成本较高; 气相色谱法对待测目标物具有局限性, 只能检测挥发性生物胺, 对于非挥发性生物胺需要进行衍生化再检测; 离子色谱法容易受金属离子的干扰, 只能检测部分生物胺; 分光光度法灵敏度较低, 且容易受到其他吸光物质的干扰; 薄层色谱法仅为半定量检测方法, 准确性较差。液相色谱法是国内外定量检测食品中生物胺最常用的方法, GB 5009.208—2016《食品安全国家标准食品中生物胺的测定》(第一法液相色谱法)中, 前处理步骤复杂、耗时长、检出限高且重复性较差, 难以满足大批量样品的日常检测需求; 此外, 该提取方法中多次氮吹步骤易造成生物胺损失, 使得加标回收率较低, 影响了实验结果的准确性。因此, 一种前处理步骤简单, 灵敏度较高, 重复性好, 适用于批量样品检验的方法亟待被开发。

鉴于此, 本研究通过优化丹磺酰氯柱前衍生生物胺的衍生反应各项条件参数, 建立可同时测定水产品中9种生物胺的高效液相色谱法, 并把所建立的方法应用于广州市售的50批次高组胺鱼类实际样品检测, 为水产品中多种生物胺的同时检测提供方法依据。

1 材料与方法

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1.1 材料与试剂

50批次高组胺鱼类(竹荚鱼、马鲛鱼、秋刀鱼、青占鱼), 来源于广州市21间市场(菜市场、农贸市场、批发市场)摊档或店铺。

色胺(纯度98.80%)、β-苯乙胺(纯度98.62%)、腐胺盐酸盐(纯度99.80%)、尸胺盐酸盐(纯度99.70%)、组胺二盐酸盐(纯度99.5%)、章鱼胺盐酸盐(纯度100.00%)、酪胺盐酸盐(纯度99.10%)、亚精胺盐酸盐(纯度99.90%)、精胺盐酸盐(纯度98.80%)、1,7-二氨基庚烷(纯度99.40%)(英国LGC公司); 丹磺酰氯(纯度99%, 上海阿拉丁生化科技股份有限公司); 三氯乙酸、氢氧化钠、丙酮(分析纯, 广州化学试剂厂); 乙腈(色谱纯, 德国默克公司); 超纯水(由上海乐枫公司超纯水仪制备)。

1.2 仪器与设备

U3000高效液相色谱仪(带二极管阵列检测器, 美国赛默飞世尔科技公司); BT125D十万分之一分析天平(德国赛多利斯公司); ME2002E百分之一分析天平(瑞士梅特勒-托利多公司); Direct-Pure UP10超纯水仪(上海乐枫公司); SW22恒温振荡水浴(德国优莱博公司); 3-30K高速冷冻离心机(德国Sigma公司); T25N-18G分散均质机(德国IKA公司); C₁₈色谱柱(250 mm×4.6 mm, 5 μm, 美国飞诺美公司)。

1.3 实验方法

1.3.1 生物胺标准溶液的配制和衍生

分别准确称取β-苯乙胺、腐胺盐酸盐、尸胺盐酸盐、组胺二盐酸盐、章鱼胺盐酸盐、酪胺盐酸盐、亚精胺盐酸盐、精胺盐酸盐标准品15~20 mg于10 mL容量瓶中, 用超纯水溶解并定容, 折算盐酸盐的质量后(其中β-苯乙胺无需折算), 分别配制得8种生物胺标准储备液(1000 mg/L), 避光4 ℃冷藏保存1个月。准确称取色胺标准品10 mg至10 mL容量瓶中, 用乙腈溶解并定容至刻度, 配制得色胺标准储备液(1000 mg/L), 避光4 ℃冷藏保存1个月。

准确称取100 mg 1,7-二氨基庚烷内标物于10 mL容量瓶中, 用超纯水溶解并定容至刻度, 配制得1,7-二氨基庚烷内标储备溶液(10 mg/mL)。

分别准确吸取适量9种生物胺标准储备液于10 mL容量瓶中, 加入10 mg/mL的1,7-二氨基庚烷内标储备液125 μL, 用超纯水定容到10 mL, 配制得质量浓度为1、10、25、50、100 mg/L(含内标125 mg/L)的生物胺标准工作溶液, 临用现配。

取300 µL各质量浓度生物胺标准溶液于2 mL离心管中, 加入40 µL 0.1 mol/L氢氧化钠溶液。避光条件下进行衍生反应, 加入600 µL 10 mg/mL丹磺酰氯丙酮溶液, 涡旋混匀, 40 ℃下衍生反应20 min, 加入100 µL氨水终止衍生反应, 涡旋混匀, 避光静置30 min, 加入460 µL乙腈, 涡旋混匀, 过0.22 μm有机相滤膜到进样瓶待上机。

1.3.2 样品的提取和衍生

取水产品样品的可食部分充分均质。准确称取5.0 g(精确至0.01 g)样品于50 mL塑料离心管中, 加入312.5 µL 10 mg/mL的1,7-二氨基庚烷内标溶液, 加入12 mL 5%三氯乙酸水溶液涡旋提取2 min, 4000 r/min离心2 min, 转移上清液至25 mL棕色容量瓶中, 再加入10 mL 5%三氯乙酸水溶液到上述50 mL塑料离心管中重复提取一次, 合并上清液, 用5%三氯乙酸水溶液定容至25 mL棕色容量瓶刻度, 混合均匀后, 取少量过膜备用。

取300 µL上述过膜样品溶液于2 mL离心管中, 加入40 µL 2 mol/L氢氧化钠溶液调节pH至9.5左右, 再加入600 µL 10 mg/mL丹磺酰氯丙酮衍生溶液, 涡旋混匀, 40 ℃下衍生反应20 min, 加入100 µL氨水终止衍生反应, 涡旋混匀, 避光静置30 min, 加入460 µL乙腈, 涡旋混匀, 过0.22 μm有机相滤膜到进样瓶待上机。

1.3.3 色谱条件

色谱柱: C₁₈ (250 mm×4.6 mm, 5 μm); 液相洗脱程序: 流动相A: 乙腈, 流动相B: 水, 流速: 0.8 mL/min, 液相梯度洗脱程序如表1所示; 紫外波长: 254 nm; 进样量: 20 µL; 柱温: 35 ℃。

1.4 数据处理

通过赛默飞公司的U3000液相色谱仪配套数据处理软件Chromeleon 7工作站系统进行数据采集及定量分析, 再利用WPS Office 2022软件进行数据分析和参数优化条形图绘制, 利用Origin 2021进行色谱图绘制。所有参数优化实验数据均设置3组平行并计算标准偏差, 方法的加标回收率及精密度试验设置6组平行并计算标准偏差。

2 结果与分析

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2.1 生物胺衍生条件的确定

2.1.1 丹磺酰氯质量浓度的确定

影响衍生反映完全程度的最重要因素之一是丹磺酰氯衍生剂的用量, 为了优化丹磺酰氯的质量浓度, 本研究使用300 μL 50 mg/L的9种生物胺混合标准溶液(含125 mg/L 1,7-二氨基庚烷内标)分别添加600 μL质量浓度为1、3、5、8、10 mg/mL的丹磺酰氯丙酮溶液进行探究。每个丹磺酰氯浓度点重复实验3次, 丹磺酰氯与生物胺的衍生物峰面积大小能反映衍生反应的完全程度。分析丹磺酰氯质量浓度对生物胺衍生物生成量的影响, 结果见图1, 9种生物胺和1,7-二氨基庚烷内标衍生物的生成量变化趋势不尽相同, 为使衍生反应彻底进行, 综合考虑所有生物胺的衍生完全程度, 选择丹磺酰氯的质量浓度为10 mg/mL。

2.1.2 衍生反应pH的确定

生物胺与丹磺酰氯的衍生反应发生在碱性条件下, 使用0.1 mol/L氢氧化钠溶液调节反应体系pH, 分别调节到8.0、8.5、9.0、9.5、10.0。每个pH在重复性条件下进行3次平行实验, 探究衍生反应体系pH对生物胺衍生物生成量的影响, 结果见图2, 生物胺衍生物的峰面积在pH 8.0~9.0基本没有变化, 当pH调节至9.5时, 生物胺衍生物的峰面积最大, 此时对应0.1 mol/L氢氧化钠溶液的使用体积为40 μL。当pH继续增大至10.0时, 生物胺衍生物的生成量下降, 因此将衍生反应的pH确定为9.5。

2.1.3 衍生反应温度的确定

探究衍生反应温度对反应完全程度的影响, 温度分别设在30、40、50、60、70 ℃。每个温度点在重复性实验条件下平行实验3次, 探究衍生反应体系的温度对生物胺衍生物生成量的影响, 结果见图3, β-苯乙胺、腐胺、尸胺、组胺衍生物的生成量随着温度的上升先增后降, 反应温度达到40 ℃时, 生物胺衍生物的峰面积最大; 章鱼胺、酪胺、亚精胺、精胺衍生物的生成量随着温度的上升而持续下降, 反应温度在30 ℃时, 生物胺衍生物的生成量最大。综合考虑9种生物胺的衍生情况, 确定最优的衍生反应温度为40 ℃。

2.1.4 衍生反应时间的确定

将衍生反应时间分别设定为10、20、30、40、50、60 min, 每个时间点在重复性实验条件下实验3次。探究衍生反应时间对生物胺衍生物生成量的影响, 结果见图4, 反应时间达到20 min时, 除章鱼胺、酪胺外, 其余7种生物胺衍生物的生成量最大。20 min后, 生物胺衍生物的生成量随着反应时间增加而逐渐下降, 由此确定最优的衍生反应时间为20 min。

以上结果表明, 衍生反应的最优条件为丹磺酰氯衍生剂质量浓度10 mg/mL、pH 9.5、温度40 ℃和反应时间20 min。

2.2 色谱图与标准工作曲线

根据上述条件优化实验确定的最优衍生反应条件以及色谱条件进样液相色谱仪分析, 50 mg/L生物胺标准品的色谱图如图5所示, 9种生物胺和1,7-二氨基庚烷内标的峰形均良好, 9种生物胺的保留时间见表2。分别配制质量浓度为1、10、25、50、100 mg/L(含内标125 mg/L)的生物胺标准溶液, 按1.3.1中的衍生方法与1.3.3中的色谱条件进行测定, 以各种生物胺与1,7-二氨基庚烷内标的色谱峰面积比值(Y)为纵坐标, 以对应的生物胺含量(X, mg/L)为横坐标, 绘制标准工作曲线。9种生物胺标准溶液在1~100 mg/L范围内, 标准曲线线性关系良好, r²均在0.9991以上, 9种生物胺的线性回归方程详见表2。

2.3 检出限和定量限

选取鱼肉阴性样品, 添加含量为5 mg/kg的标准溶液, 按照1.3.2的方法提取和衍生后, 按照1.3.3的色谱条件上机检测。以信噪比S/N=3计算获得的含量为检出限, 信噪比S/N=10计算获得的含量为定量限, 9种生物胺的检出限和定量限信息详见表2。结果显示, 本研究方法的9种生物胺检出限在0.32~2.28 mg/kg, 定量限在1.08~7.59 mg/kg, 相较于GB 5009.208—2016液相色谱法的检出限20 mg/kg和定量限50 mg/kg, 本研究方法在灵敏度上有显著提高。

2.4 方法的加标回收率和精密度

选择竹荚鱼、马鲛鱼、秋刀鱼、青占鱼阴性鱼肉样品做9种生物胺的加标回收实验, 添加定量限1、2、5倍的9种生物胺, 在重复性实验条件下平行实验6次, 方法的加标回收率和精密度详见表3, 空白样品色谱图与加标样品色谱图见图6。

9种生物胺的加标回收率在85.2%~106.7%之间, 精密度在1.5%~4.9%之间。方法的加标回收率和精密度能满足方法学的验证要求, 可适用于日常实验的批量测定。

2.5 与国标方法的比对实验

选择竹荚鱼、马鲛鱼、秋刀鱼、青占鱼阴性鱼肉样品各1批次, 加入9种生物胺各100 mg/kg, 分别采用本研究方法和GB 5009.208—2016(第一法液相色谱法)进行加标回收比对实验, 在重复性实验条件下平行实验6次, 两个方法的加标回收率和精密度详见表4。

在100 mg/kg的加标水平下, 9种生物胺国标法的加标回收率在81.6%~103.8%之间, 精密度在7.4%~9.8%之间; 本研究方法的加标回收率在93.0%~104.7%之间, 精密度在1.9%~3.8%之间。结果显示, 采用GB 5009.208—2016与本研究方法做加标回收实验, 加标回收率均落在合理范围, 两个方法的9种生物胺含量结果一致。本研究方法的加标回收率比国标法高, 精密度比GB 5009.208—2016好, 这是由于本研究方法减少了多次氮吹等复杂的前处理步骤, 使得目标物损失更少、方法更精密。国标法前处理时间达300 min, 本研究方法前处理在80 min内可完成, 本方法更为简单便捷, 能有效减少前处理时间。

2.6 方法的实际应用

采用该方法测定了50批次高组胺鱼类(12批次竹荚鱼、12批次马鲛鱼、12批次秋刀鱼、14批次青占鱼)中9种生物胺的含量。

结果显示, 6批次马鲛鱼、2批次青占鱼、11批次秋刀鱼、6批次竹荚鱼的9种生物胺均未检出, 另外25批次的高组胺鱼类样品中至少有一种生物胺检出, 检出情况见表5。 50批次市售高组胺鱼类中, β-苯乙胺有15批次检出, 含量在24.0~34.1 mg/kg, 青占鱼检出率最高, 其次为竹荚鱼、秋刀鱼; 腐胺有2批次检出, 分别为马鲛鱼1批次26.2 mg/kg, 青占鱼1批次16.0 mg/kg; 尸胺有13批次检出, 含量在13.1~32.2 mg/kg, 马鲛鱼检出率最高, 青占鱼其次, 然后是秋刀鱼; 酪胺有2批次检出, 含量在10.0~15.2 mg/kg, 均为马鲛鱼。50批次高组胺鱼类样品的色胺、组胺、章鱼胺、亚精胺、精氨均为未检出。

3 结论

收起

本研究采用丹磺酰氯柱前衍生-反相液相色谱法测定水产品中的9种生物胺, 优化确定丹磺酰氯衍生溶液的质量浓度为10 mg/mL, 衍生反应pH为9.5, 衍生反应温度为40 ℃, 衍生反应时间为20 min。9种生物胺的加标回收率在85.2%~106.7%之间, 精密度在1.5%~4.9%之间, 方法的加标回收率和精密度能满足方法学的验证要求。方法较GB 5009.208—2016(第一法液相色谱法)步骤简便、快速且灵敏度显著提高, 9种生物胺定量限从50 mg/kg下降至1.08~7.59 mg/kg, 可适用于水产品中9种生物胺的批量样品测定。

基金

收起

广州检验检测认证集团有限公司科技项目(2019kj07GZ)

参考文献

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doi: 10.19812/j.cnki.jfsq11-5956/ts.20241018004

接收时间：2024-10-18
首发时间：2025-07-19
出版时间：2025-03-15

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收稿日期：2024-10-18

基金

广州检验检测认证集团有限公司科技项目(2019kj07GZ)

作者信息

1.广州检验检测认证集团有限公司, 广州 511447

2.国家加工食品质量检验检测中心(广东), 广州 511447

通讯作者:

^* 李秀英(1984—), 女, 硕士, 高级工程师, 主要研究方向为食品质量安全分析检测。E-mail: 328444798@qq.com

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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组成	时间/min
流动相A/%	58	78	90	90	58	58
流动相B/%	42	22	10	10	42	42

组成

时间/min

0.00

22.00

25.00

32.00

32.01

37.00

流动相A/%

流动相B/%

化合物	保留时间/min	线性方程	r²	检出限/(mg/kg)	定量限/(mg/kg)
色胺	13.3	Y=2.1263X-1.0603	0.9992	0.93	3.10
β-苯乙胺	15.6	Y=2.1228X-2.2119	0.9993	1.05	3.51
腐胺	17.0	Y=4.2678X-2.2157	0.9998	0.32	1.08
尸胺	18.5	Y=3.7806X-2.5078	0.9995	0.38	1.28
组胺	19.7	Y=2.1383X+1.5954	0.9999	0.69	2.31
章鱼胺	20.9	Y=2.1103X+1.4512	0.9991	1.22	4.06
酪胺	26.6	Y=2.2038X+1.9809	0.9995	0.97	3.25
亚精胺	28.0	Y=2.1319X+1.8553	0.9995	0.96	3.19
精氨	33.0	Y=2.0865X+1.5730	0.9992	2.28	7.59

化合物

保留时间/min

线性方程

r²

检出限/(mg/kg)

定量限/(mg/kg)

色胺

13.3

Y=2.1263X-1.0603

0.9992

0.93

3.10

β-苯乙胺

15.6

Y=2.1228X-2.2119

0.9993

1.05

3.51

腐胺

17.0

Y=4.2678X-2.2157

0.9998

0.32

1.08

尸胺

18.5

Y=3.7806X-2.5078

0.9995

0.38

1.28

组胺

19.7

Y=2.1383X+1.5954

0.9999

0.69

2.31

章鱼胺

20.9

Y=2.1103X+1.4512

0.9991

1.22

4.06

酪胺

26.6

Y=2.2038X+1.9809

0.9995

0.97

3.25

亚精胺

28.0

Y=2.1319X+1.8553

0.9995

0.96

3.19

精氨

33.0

Y=2.0865X+1.5730

0.9992

2.28

7.59

化合物	1倍定量限	2倍定量限	5倍定量限
色胺	89.6~103.5	2.8~4.6	87.8~104.6	2.3~4.4	88.6~105.8	2.9~4.0
β-苯乙胺	86.5~105.4	2.6~4.5	87.8~102.1	2.6~4.9	90.9~103.6	2.2~4.7
腐胺	87.5~104.6	1.5~3.6	86.3~105.7	2.1~4.7	88.1~104.3	2.5~4.9
尸胺	85.2~104.3	1.9~4.7	86.9~105.1	1.9~4.0	89.6~106.5	1.8~4.5
组胺	90.1~102.3	2.7~4.9	87.9~102.6	2.4~4.6	89.5~102.4	2.0~4.8
章鱼胺	92.1~105.2	1.8~4.5	92.7~106.7	1.9~4.8	91.1~105.1	2.2~4.6
酪胺	90.8~103.5	2.1~4.6	91.2~103.2	3.2~4.9	92.2~103.4	3.1~4.8
亚精胺	86.5~102.1	1.9~4.0	85.6~103.5	2.0~4.8	86.9~102.5	1.7~4.6
精胺	92.1~103.5	2.5~4.8	91.2~104.5	2.2~4.6	93.0~104.3	2.4~4.9

化合物

1倍定量限

2倍定量限

5倍定量限

加标回收率

RSDs

加标回收率

RSDs

加标回收率

RSDs

色胺

89.6~103.5

2.8~4.6

87.8~104.6

2.3~4.4

88.6~105.8

2.9~4.0

β-苯乙胺

86.5~105.4

2.6~4.5

87.8~102.1

2.6~4.9

90.9~103.6

2.2~4.7

腐胺

87.5~104.6

1.5~3.6

86.3~105.7

2.1~4.7

88.1~104.3

2.5~4.9

尸胺

85.2~104.3

1.9~4.7

86.9~105.1

1.9~4.0

89.6~106.5

1.8~4.5

组胺

90.1~102.3

2.7~4.9

87.9~102.6

2.4~4.6

89.5~102.4

2.0~4.8

章鱼胺

92.1~105.2

1.8~4.5

92.7~106.7

1.9~4.8

91.1~105.1

2.2~4.6

酪胺

90.8~103.5

2.1~4.6

91.2~103.2

3.2~4.9

92.2~103.4

3.1~4.8

亚精胺

86.5~102.1

1.9~4.0

85.6~103.5

2.0~4.8

86.9~102.5

1.7~4.6

精胺

92.1~103.5

2.5~4.8

91.2~104.5

2.2~4.6

93.0~104.3

2.4~4.9

化合物	GB 5009.208—2016	本研究方法
色胺	82.3~101.3	7.9~9.8	94.6~103.6	2.3~3.1
β-苯乙胺	85.2~102.1	7.4~9.5	94.0~104.2	2.0~3.2
腐胺	81.6~101.0	8.0~9.7	93.9~102.9	1.9~3.8
尸胺	82.9~103.2	7.7~9.6	93.0~104.6	1.9~3.3
组胺	86.5~102.7	7.6~9.4	95.6~103.9	2.5~3.6
章鱼胺	82.5~103.8	7.5~9.6	93.6~103.4	2.3~3.8
酪胺	83.5~102.4	7.4~9.3	94.2~104.7	2.0~3.5
亚精胺	82.4~103.1	7.6~9.7	94.1~104.1	2.3~3.7
精胺	83.4~102.8	8.2~9.8	94.8~103.9	2.4~3.7

化合物

GB 5009.208—2016

本研究方法

加标回收率

RSDs

加标回收率

RSDs

色胺

82.3~101.3

7.9~9.8

94.6~103.6

2.3~3.1

β-苯乙胺

85.2~102.1

7.4~9.5

94.0~104.2

2.0~3.2

腐胺

81.6~101.0

8.0~9.7

93.9~102.9

1.9~3.8

尸胺

82.9~103.2

7.7~9.6

93.0~104.6

1.9~3.3

组胺

86.5~102.7

7.6~9.4

95.6~103.9

2.5~3.6

章鱼胺

82.5~103.8

7.5~9.6

93.6~103.4

2.3~3.8

酪胺

83.5~102.4

7.4~9.3

94.2~104.7

2.0~3.5

亚精胺

82.4~103.1

7.6~9.7

94.1~104.1

2.3~3.7

精胺

83.4~102.8

8.2~9.8

94.8~103.9

2.4~3.7

样品名称	色胺	β-苯乙胺	腐胺	尸胺	组胺	章鱼胺	酪胺	亚精胺	精胺
马鲛鱼1	N.D.	N.D.	N.D.	32.2	N.D.	N.D.	10.0	N.D.	N.D.
马鲛鱼2	N.D.	N.D.	N.D.	24.9	N.D.	N.D.	N.D.	N.D.	N.D.
马鲛鱼3	N.D.	N.D.	26.2	N.D.	N.D.	N.D.	15.2	N.D.	N.D.
马鲛鱼4	N.D.	N.D.	N.D.	13.1	N.D.	N.D.	N.D.	N.D.	N.D.
马鲛鱼5	N.D.	N.D.	N.D.	15.1	N.D.	N.D.	N.D.	N.D.	N.D.
马鲛鱼6	N.D.	N.D.	N.D.	15.0	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼1	N.D.	34.1	N.D.	19.7	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼2	N.D.	26.7	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼3	N.D.	25.1	N.D.	18.0	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼4	N.D.	30.3	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼5	N.D.	25.8	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼6	N.D.	26.1	16.0	18.1	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼7	N.D.	28.6	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼8	N.D.	26.2	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼9	N.D.	27.8	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼10	N.D.	27.1	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼11	N.D.	N.D.	N.D.	13.2	N.D.	N.D.	N.D.	N.D.	N.D.
青占鱼12	N.D.	27.3	N.D.	13.7	N.D.	N.D.	N.D.	N.D.	N.D.
秋刀鱼1	N.D.	24.0	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼1	N.D.	N.D.	N.D.	20.2	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼2	N.D.	N.D.	N.D.	14.8	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼3	N.D.	N.D.	N.D.	15.7	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼4	N.D.	28.2	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼5	N.D.	29.2	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
竹荚鱼6	N.D.	29.6	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.

样品名称

色胺

β-苯乙胺

腐胺

尸胺

组胺

章鱼胺

酪胺

亚精胺

精胺

马鲛鱼1

N.D.

32.2

N.D.

10.0

N.D.

马鲛鱼2

N.D.

24.9

N.D.

马鲛鱼3

N.D.

26.2

N.D.

15.2

N.D.

马鲛鱼4

N.D.

13.1

N.D.

马鲛鱼5

N.D.

15.1

N.D.

马鲛鱼6

N.D.

15.0

N.D.

青占鱼1

N.D.

34.1

N.D.

19.7

N.D.

青占鱼2

N.D.

26.7

N.D.

青占鱼3

N.D.

25.1

N.D.

18.0

N.D.

青占鱼4

N.D.

30.3

N.D.

青占鱼5

N.D.

25.8

N.D.

青占鱼6

N.D.

26.1

16.0

18.1

N.D.

青占鱼7

N.D.

28.6

N.D.

青占鱼8

N.D.

26.2

N.D.

青占鱼9

N.D.

27.8

N.D.

青占鱼10

N.D.

27.1

N.D.

青占鱼11

N.D.

13.2

N.D.

青占鱼12

N.D.

27.3

N.D.

13.7

N.D.

秋刀鱼1

N.D.

24.0

N.D.

竹荚鱼1

N.D.

20.2

N.D.

竹荚鱼2

N.D.

14.8

N.D.

竹荚鱼3

N.D.

15.7

N.D.

竹荚鱼4

N.D.

28.2

N.D.

竹荚鱼5

N.D.

29.2

N.D.

竹荚鱼6

N.D.

29.6

N.D.