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Applied Biological Chemistry

Table 4 Linearities, LODs, LOQs, recoveries, and RSDs obtained by LC–MS/MS analysis method in Lithospermi Radix

From: A LC–ESI–MS/MS analysis procedure coupled with solid phase extraction and MeOH extraction method for determination of pyrrolizidine alkaloids in Tussilago farfara and Lithospermi erythrorhzion

No.

Pyrrolizidine alkaloids

Range (ng/mL)

Linearity (r2)

LOD (μg/kg)

LOQ (μg/kg)

Recovery (%) mean ± SD, n = 3

Intra-day RSDb (%)

Inter-day RSD (%), n = 9

Low level

Medium level

High level

1

Echimidine

2.0–200

0.999

–

–

108.9 ± 3.3

108.5 ± 7.2

115.2 ± 3.6

4.2

2.6

2

Echimidine N-oxide

2.0–200

0.999

–

–

123.1 ± 5.4

118.6 ± 4.8

130.3 ± 4.4

3.9

4.2

3

Erucifoline

1.0–40

0.999

0.3

0.8

81.4 ± 4.3

83.6 ± 6.9

87.0 ± 4.6

9.5

4.2

4

Erucifoline N-oxide

1.0–40

0.999

0.5

1.5

102.0 ± 6.0

102.8 ± 14.6

116.5 ± 3.6

4.1

3.6

5

Europine

0.5–20

0.999

0.4

1.1

97.3 ± 7.2

95.1 ± 8.2

97.5 ± 7.4

6.4

9.0

6

Europine N-oxide

0.5–20

0.999

0.6

1.7

104.5 ± 7.0

98.5 ± 9.7

108.2 ± 5.5

24.2

13.8

7

Heliotrine

0.5–20

0.999

1.0

3.0

92.4 ± 5.0

92.0 ± 3.8

91.6 ± 6.0

9.0

25.2

8

Heliotrine N-oxide

0.5–20

0.999

0.2

0.7

110.9 ± 5.8

101.5 ± 13.6

112.5 ± 6.3

4.4

9.0

9

Intermedine

2.0–200

0.999

–a

–

111.1 ± 3.7

111.7 ± 14.4

116.6 ± 5.7

7.0

7.6

10

Intermedine N-oxide

2.0–200

0.999

–

–

119.7 ± 6.2

118.3 ± 16.2

119.6 ± 4.7

7.6

9.4

11

Jacobine

1.0–40

0.999

0.7

2.2

71.4 ± 4.0

72.3 ± 4.7

74.9 ± 3.9

18.5

9.4

12

Jacobine N-oxide

1.0–40

0.999

0.1

0.4

107.0 ± 6.2

106.3 ± 7.1

116.2 ± 5.9

2.6

2.6

13

Lasiocarpine

0.5–20

0.999

0.2

0.6

79.6 ± 5.4

84.6 ± 3.2

79.4 ± 3.8

9.9

10.7

14

Lasiocarpine N-oxide

1.0–40

0.999

0.8

2.3

106.7 ± 5.8

95.4 ± 12.7

105.4 ± 6.3

7.4

5.8

15

Lycopsamine

0.5–20

0.999

2.4

7.2

109.2 ± 7.7

102.4 ± 6.3

97.5 ± 5.3

11.1

11.7

16

Lycopsamine N-oxide

2.0–80

0.999

–

–

93.0 ± 8.0

82.7 ± 16.1

112.2 ± 8.4

11.4

21.0

17

Monocrotaline

0.5–20

0.999

0.6

1.8

95.8 ± 5.4

104.3 ± 4.8

82.4 ± 3.1

4.3

7.9

18

Monocrotaline N-oxide

1.0–40

0.999

0.6

1.8

104.4 ± 5.9

95.0 ± 14.7

108.0 ± 5.8

8.7

11.0

19

Retrorsine

1.0–40

0.999

0.7

2.1

80.8 ± 6.5

81.0 ± 4.3

80.8 ± 6.1

6.0

11.3

20

Retrorsine N-oxide

2.0–80

0.999

5.8

17.4

110.1 ± 5.6

105.0 ± 12.2

115.8 ± 6.1

7.8

18.3

21

Senecionine

0.5–20

0.999

0.4

1.1

73.8 ± 3.3

70.2 ± 3.8

77.2 ± 5.8

5.0

9.0

22

Senecionine N-oxide

1.0–40

0.999

0.9

2.8

107.8 ± 4.4

105.1 ± 10.8

114.8 ± 6.5

7.8

13.4

23

Seneciphylline

2.0–80

0.999

7.7

23.0

70.4 ± 2.9

73.0 ± 4.5

75.0 ± 4.7

9.0

19.8

24

Seneciphylline N-oxide

1.0–40

0.999

0.4

1.2

82.0 ± 4.9

81.9 ± 7.4

86.1 ± 5.5

8.2

2.6

25

Senecivernine

0.5–20

0.999

0.4

1.2

73.0 ± 3.4

71.0 ± 3.5

70.6 ± 4.3

8.3

18.0

26

Senecivernine N-oxide

1.0–40

0.999

0.4

1.1

101.9 ± 4.0

103.1 ± 5.2

105.8 ± 7.2

3.6

2.0

27

Senkirkine

0.5–20

0.999

0.1

0.2

94.8 ± 6.6

102.0 ± 3.9

100.3 ± 7.5

10.8

15.5

28

Trichodesmine

0.5–20

0.999

0.3

1.0

83.2 ± 4.6

85.9 ± 3.8

80.6 ± 6.2

4.3

5.4

  1. aNot available because saturation occurred by high content of the PA contained in in the Lithospermi Radix
  2. bRSD relative standard deviation
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