10

DB36

T

1841—2023土壤

3

種四環(huán)素類抗生素的測(cè)定

高效液相色譜-三重四極桿質(zhì)譜法Determination

of

three

tetracycline

antibiotics

by

high

performance

liquidchromatography-triple

mass

spectrometry2023

-

09

-

18

發(fā)布2024

-

-

01

實(shí)施江西省市場(chǎng)監(jiān)督管理局 發(fā)

布

18412023

II

10

11

12

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

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

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

11

1841本文件按照

《標(biāo)準(zhǔn)化工作導(dǎo)則第部分：標(biāo)準(zhǔn)化文件的結(jié)構(gòu)和起草規(guī)則》的規(guī)定起

18412023

高校液相色譜

613

166

使用乙腈與緩沖液，經(jīng)水平振蕩提取土壤樣品中四環(huán)素類抗生素，提取液經(jīng)冷凍

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

離心管中，加入樣品提取液（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種不同濃度的溶液，1.00

20.0

50.0

100

200

500

標(biāo)準(zhǔn)8.3

取按（7.2）制備好的待測(cè)試樣，按照與繪制校準(zhǔn)曲線相同的儀器分析條件進(jìn)行測(cè)定。當(dāng)待測(cè)試樣8.4

(7.2)8.1

>5020≤5025≤2030≤1050

18419.1

2.5

表4

圖1

9.2

184120239.3

當(dāng)測(cè)定結(jié)果大于等于

時(shí)，數(shù)據(jù)保留三位有效數(shù)字；當(dāng)結(jié)果小于

時(shí)，保留至小數(shù)點(diǎn)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

；四環(huán)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個(gè)基體加標(biāo)樣，加標(biāo)樣與原樣品在完全相同的測(cè)試條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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Adv,2019,9(5):15686

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,2019,38(2):194200

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