Figure 1 Ascorbic acid and sodium nitrite effect on nitrosamine formation in during time

No.

Name

Polarity

Boiling point (°C)

CAS

1

N-Nitrosodimethylamine (NDMA)

log Kow*= -0.57

154.0

62-75-9

2

N-Nitrosomethylethylamine (NMEA)

log Kow = 0.04

170.0

10595-95-6

3

N-Nitrosodiethylamine (NDEA)

log Kow = 0.48

176.9

55-18-5

4

N-Nitrosodi-n-propylamine (NDPA)

log Kow= 1.360

206.0

621-64-7

5

N-Nitrosodibutylamine (NDBA)

log Kow = 2.63

237.0

924-16-3

6

N-Nitrosodiphenylamine (NDPhA)

Log Kow= 3.13

268.0

86-30-6

7

1-Nitrosopiperidine (NPIP)

log Kow = 0.36

219.0

100-75-4

8

1-Nitrosopyrrolidine (NPYR)

log Kow = -0.19

214.0

930-55-2

9

Nitrosomorpholine (NMOR)

log Kow = -0.44

225.0

59-89-2

*Kow's have redistributed from,30

Table 1. Nitrosamines specifications

Operating parameters

Values

Injection volume (µL)

2

Inlet temperature (oC)

280

Flow (ml min-1)

1.0

Temperature programming

5 min isothermal at 60 °C, programmed to rise at 5 °C min-1 to 160 °C, rise at 20 °C min-1 to 240 °C,15 min isothermal at 240 °C

Detector temperature (oC)

300

Makeup-gas flow (N2) (mL min−1)

20

Carrier gas

Nitrogen

Mode

Pulsed splitless - Constant flow

Table 2. Typical operating conditions for GC-FID.

Performance Characteristics

Nitrosamine

RT

Linear dynamic range, LDR (mg L-1)

The determination coefficient (R2)

Limit of detection, LOD
μg kg-1

Limit of quantification, LOQ
μg kg-1

Relative standard deviation, RSD (%)

NDMA

11.5

1.0-10

0.997

0.4

1.0

7.2

NMEA

12.6

1.0-10

0.989

0.4

1.0

8.6

NDEA

13.3

1.0-10

0.988

0.4

1.0

8.2

NDPA

16.7

1.0-10

0.984

0.4

1.0

10.5

NDBA

21.0

2.0-10

0.982

0.7

2.0

11.7

NDPhA

21.4

1.0-10

0.990

0.4

1.0

5.0

NPIP

22.2

2.0-10

0.995

0.7

2.0

6.7

NPYR

23.4

1.0-10

0.992

0.4

1.0

4.2

NMOR

31.1

1.0-10

0.993

0.4

1.0

4.2

Table 3: Analytical performance data for nitrosamines determination.

N-nitrosamine

Spiked Level(μg/L)

Raw sausage

Fried sausage

Recovery

%RSD

Recovery

%RSD

NDMA

1

5

10

70

85

95

5

4

3

72

83

97

5

4

3

NMEA

1

5

10

68

87

92

5

5

3

70

85

95

6

4

5

NDEA

1

5

10

71

85

95

4

5

3

68

85

95

6

3

4

NDPA

1

5

10

70

85

95

6

4

3

67

83

96

4

4

3

NDBA

5

10

85

92

5

3

85

95

4

3

NDPhA

1

5

10

77

80

93

3

5

7

75

84

90

5

6

3

NPIP

5

10

88

94

6

3

85

97

7

5

NPYR

1

5

10

63

75

89

5

6

3

66

78

93

4

8

4

NMOR

1

5

10

71

86

92

6

4

3

74

88

96

7

5

2

Table 4: Results of recoveries for nine spiked nitrosamines in sausage samples (n = 3).

Ref.

Linear range

(µg Kg-1)

Real sample

Recovery

(%)

Detection Limit

(µg Kg-1)

Quantitation limit (µg Kg-1)

Method

[3]

0.25-500

Fast food, meat

82-105.5

0.077-0.18

0.26 to 0.6

GC-NCD

[35]

-

Potato

103

0.001

0.003

GC-EID

[18]

-

Sausages

20-81.6

-

400

SFE and MEKC

[36]

10000-200000

Water

82-111

400-1600

0.13

GC-MS-PCI

[6]

0.25-500

Meat products

60-105

0.01-0.12

0.03-0.36

SPE-GC-CI-MS

[3]

2-300

Meat products

76-85

1.66–3.86

6.96-16.71

GC-GC-NCD

[7]

-

Foodstuff

80-120

0.10-0.30

-

GC-PCI-MS/MS

[1]

1-100

Processed meats

70-114

0.15-0.37

0.5-1.24

GC-MCI-MS

[28]

5-50

Food

80-110

0.03-1.26

0.08-2.76

HPLC-APCI-MS/MS

[37]

0.3-100

Food products

74-117

0.08-0.55

0.26-1.82

HPLC-UV

[38]

1-100

Processed meats

70-114

0.15-0.37

0.50-1.24

GC-CI-MS

[27]

0.1-100

Water

97.44-107.16

0.00078-0.0112

 

HS-SPME-GC-MS

This work

50-500000

Sausage

63-97

0.4

0.5-1.0

GC-FID

Table 5: Method analytical figures of merit for nitrosamines determination in sausage at a comparison to other methods