DB36-T 1841-2023 土壤3种四环素类抗生素的测定高效液相色谱-三重四极杆质谱法

10

DB36

T

1841—2023土壤

3

种四环素类抗生素的测定

高效液相色谱-三重四极杆质谱法Determination

of

three

tetracycline

antibiotics

by

high

performance

liquidchromatography-triple

mass

spectrometry2023

-

09

-

18

发布2024

-

-

01

实施江西省市场监督管理局 发

布

18412023

II

10

11

12

................................................

........................................

.........................................................10

11

1841本文件按照

《标准化工作导则第部分：标准化文件的结构和起草规则》的规定起

18412023

高校液相色谱

613

166

使用乙腈与缓冲液，经水平振荡提取土壤样品中四环素类抗生素，提取液经冷冻

5.1

5.2

5.3

5.1

5.4

5.5

5.6

5.7

0.1

1.0

1000

5.8

0.1

1.0

1000

5.9

99%5.10 100

5.9），5.5

100

18415.11100

5.105.5

100

5.12

27.6

12.9

37.2

350

500

5.13

5.14

5.15

6.1

6.2

0.0001g6.3

6.4

6.5

2.1

6.6

6.7

6.8

10

20

50

100

μL6.9

6.10

7.1

7d30d7.2

48h

HJ

613

2.0

50

mL

离心管中，加入样品提取液（5.12）10

45

10

min

200

mL

甲醇（5.5）、3

mL

0.5

mL

HLB

mL

mL

30

mL

mL

mL

0.22

9010901040609590100.1

4.60.1

4.70.2

30

2.0

ESI4000

35

psi10

184120238.1

表1

表2

8.2

5.115.5种不同浓度的溶液，1.00

20.0

50.0

100

200

500

标准8.3

取按（7.2）制备好的待测试样，按照与绘制校准曲线相同的仪器分析条件进行测定。当待测试样8.4

(7.2)8.1

>5020≤5025≤2030≤1050

18419.1

2.5

表4

图1

9.2

184120239.3

当测定结果大于等于

时，数据保留三位有效数字；当结果小于

时，保留至小数点后10

10.15.00

50.0

200

5.1

3.5

3.0

5.5

3.6

2.9

6.6

3.2

3.3

10.2 5.00

50.0

200

118

82.0

112

80.5

103

:92.8

100

87.9

113

93.8

102

；四环素95.4

116

86.9

111

79.6

118

11

11.1 11.2

r≥0.995

20

20

≤25%11.32020≤20%11.4

18412020个基体加标样，加标样与原样品在完全相同的测试条70

120

12

0.20.8

0.20.8

0.20.8

18412023

5.00

50.0

20.0

50.0

5.00

50.0

20.0

50

9.61.66.11.91.7281.67.65.11112242822

1.810.02.38.21.74.426125.49.07.0127.0

1.8111.45.91.84.027105.89.014121910

5.00

50.0

20.0

50.0

5.00

50.0

20.0

50.0

0.716.80.75.416.817.017.311.637.718.7

0.916.40.96.616.414.019.63.017.619.0

1.119.81.15.419.813.520.25.317.320.7

18412023

5.00

50.0

100.2±2295.195.4±1894.694.6±1897.899.899.8±1897.3102.7±1697.197.1±1896.81496.8±2820.0

50.0

105.099.099±14102.51294.694.6±1091.21091.2±2096.31096.3±2094.21094.2±20

18412023

/V/V

443.9*153.91830

461.1425.9*200.91442

445.1410*14,26

1841

10DB36/T

18412023

,2012

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and

and

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and

10

newapproach

of

of

chemistry,2018,410:1697

20

1679

and

of

and

northern

Adv,2019,9(5):15686

等．19

,2019,38(2):194200

,2