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λã>xxYӍ>˜>ˎOPڌyƷмɷֵęzyͻyƷпȾˎęzy{뻯yƷȫgҎ2015棩ͨ棨2019 66̖

ˎOPڌyƷмɷֵęzyͻyƷпȾˎęzy{뻯yƷȫgҎ2015棩ͨ棨2019 66̖

2019/9/30݋Ma Liang ˚⣺1194


   2019927գˎƷO־WվlˎOPڌyƷмɷֵęzyͻyƷпȾˎęzy{뻯yƷȫgҎ2015棩ͨ棨2019 66̖ͨQˎƷOֽMˡyƷмɷֵęzy͡yƷпȾˎęzyyƷ˜ʌίTȫwhhͨ^F԰l2.342.35헼{롶yƷȫgҎ2015棩¡ 

һ

yƷмɷֵęzy

Determination of Hormone Components in Cosmetics

 

1

Ҏ˲øЧҺɫV-|VyyƷеļɷ֣c

mڸ˪ҺҺBˮҺBͻzĤȻyƷмɷֵĶc

2 Ҫ

Ʒ܄ȡøЧҺɫVxx|VzyzyrgxӌSȱȶԡxӌeԘ˜Ӌ㺬

63Nɷֵęzޡ޺ȡ0.2 gręzȡͶҊ1

1  63NɷֵęzޡޡzȺͶ

̖

Q

ӢQ

μg/g

Ͷȣμg/g

ng/mL

ޣng/mL

1

Triamcinolone

0.03

0.1

0.6

2

2

Prednisolone

0.03

0.1

0.6

2

3

Prednisone

0.03

0.1

0.6

2

4

9-fluoroprednisolone

0.03

0.1

0.6

2

5

仯ɵ

Hydrocortisone

0.03

0.1

0.6

2

6

ɵ

Cortisone

0.03

0.1

0.6

2

7

׻

Methylprednisolone

0.03

0.1

0.6

2

8

Betamethasone

0.03

0.1

0.6

2

9

Dexamethasone

0.03

0.1

0.6

2

10

Flumethasone

0.03

0.1

0.6

2

11

Beclomethasone

0.03

0.1

0.6

2

12

ε

Triamcinolone acetonide

0.03

0.1

0.6

2

13

ε

Desonide

0.03

0.1

0.6

2

14

s

Flunisolide

0.03

0.1

0.6

2

15

p

Fluocinolone acetonide

0.03

0.1

0.6

2

16

p

Triamcinolone diacetate

0.03

0.1

0.6

2

17

s

Fludroxycortide

0.1

0.3

2

6

18

Prednisolone 21-acetate

0.03

0.1

0.6

2

19

Fluoromethalone

0.03

0.1

0.6

2

20

仯ɵɴ

Hydrocortisone 21-acetate

0.03

0.1

0.6

2

21

ɵɴ

Fludrocortisone 21-acetate

0.03

0.1

0.6

2

22

ط

Deflazacort

0.03

0.1

0.6

2

23

ɴ

Prednisone 21-acetate

0.03

0.1

0.6

2

24

ɵɴ

Cortisone 21-acetate

0.03

0.1

0.6

2

25

u

Halometasone

0.1

0.3

2

6

26

׻

Methylprednisolone 21-acetate

0.03

0.1

0.6

2

27

ɴ

Betamethasone 21-acetate

0.03

0.1

0.6

2

28

Testosterone

0.03

0.1

0.6

2

29

ɴ

Dexamethasone 21-acetate

0.03

0.1

0.6

2

30

ε

Budesonide

0.03

0.1

0.6

2

31

仯ɵɶ

Hydrocortisone 17-butyrate

0.03

0.1

0.6

2

32

ϩͪ

Gestrinone

0.03

0.1

0.6

2

33

Fluorometholone 17-acetate

0.03

0.1

0.6

2

34

׻Gͪ

Methyltestosterone

0.03

0.1

0.6

2

35

仯ɵ

Hydrocortisone 17-valerate

0.03

0.1

0.6

2

36

ε´

Triamcinolone acetonide acetate

0.03

0.1

0.6

2

37

p

Diflorasone diacetate

0.03

0.1

0.6

2

38

Fluocinonide

0.03

0.1

0.6

2

39

ȲZͪ

Norgestrel

0.03

0.1

0.6

2

40

Betamethasone 17-valerate

0.03

0.1

0.6

2

41

ε

Halcinonide

0.1

0.3

2

6

42

Prednicarbate

0.03

0.1

0.6

2

43

杊Z

Loteprednol etabonate

0.03

0.1

0.6

2

44

p

Alclomethasone dipropionate

0.03

0.1

0.6

2

45

ε

Amcinonide

0.03

0.1

0.6

2

46

u

Halobetasol Propionate

0.03

0.1

0.6

2

47

ȱ

Clobetasol 17-propionate

0.03

0.1

0.6

2

48

濨ɱ

Fluticasone propionate

0.03

0.1

0.6

2

49

Īɿ

Mometasone furoate

0.03

0.1

0.6

2

50

׵ͪ

Megestrol acetate

0.03

0.1

0.6

2

51

ȵͪ

Chlormadinone acetate

0.03

0.1

0.6

2

52

p

Betamethasone dipropionate

0.03

0.1

0.6

2

53

Swͪ

Progesterone

0.03

0.1

0.6

2

54

Medroxyprogesterone 17-acetate

0.03

0.1

0.6

2

55

p

Beclmetasone dipropionate

0.03

0.1

0.6

2

56

p

Diflucortolone valerate

0.03

0.1

0.6

2

57

ȱɶ

Clobetasone 17-butyrate

0.03

0.1

0.6

2

58

Hydroxyprogesterone caproate

0.03

0.1

0.6

2

59

Ciclesonide

0.03

0.1

0.6

2

60

Estriol

0.1

0.3

2

6

61

ƶ

Estradial

0.1

0.3

2

6

62

ͪ

Estrone

0.1

0.3

2

6

63

ϩƷ

Diethylstilbestrol

0.03

0.1

0.6

2

3 ԇͲ

Ҏ⣬ԇҎˮGB/T 6682Ҏһˮ

3.1 棺ɫV

3.2 飺ɫV

3.3 50%Һȡ桢ˮweϣu

3.4 70%Һȡ桢ˮwe7:3ϣu

3.5ƣ

Aˮ

B3.1

3.6˜ʃҺ

քeQȡؘ˜Ʒ110 mg_0.00001 g50 mLƿУ棨3.1ʹܽⲢ̶ȡ

4 xO

4.1ҺɫV-ĘOU|V“Ãx

4.2ƽ

4.3xęC

4.4•ϴx

4.5uσx

5 E

5.1Ϙ˜ҺƂ

քeȡؘ˜ʃҺ3.6m50%Һ3.3Ƴɝڶ޸Һ

עɷă܉򱣳փxɫVl|Vyȷl̶yָجFãS|ؘ˜ƷҺ63NػϘ˜ƷҺlķԡY؏MпơlăxɫVl|VlrŒMMжλ

|ؘ˜ʃҺQȡε¡uɡε¡ɡɴsɡȱhε¡ƶϩƷӘ˜Ʒs10 mg_0.00001 g100 mLƿУ棨3.1ܽⲢ̶ȣ|ؘ˜ʃҺ-20档|V푑^ijɷ֣ҿԓɷ|ؘ˜|ߺYʴ_ԡ

|ؘ˜ʻҺքeȡ|ؘ˜ʃҺm50%Һ3.3Ƴɝڶ޸Һ

5.2 Ʒ̎

5.2.1 ˪ҺҺBˮzĤƷ

QȡƷ0.2 g_0.001g10 mLɫУ棨3.1ڜuσxʎ30sԇcȡ܄ϾȻ̶ȣ•ȡ20 minoҜأ棨3.1̶ȣu4000 r/minx10 minV^ҪrȡҺm50%Һ3.3ϡጣϡҺ0.22 μmVĤ^VVҺyҺ

5.2.2 ҺBͻ

QȡƷ0.2 g_0.001gxĹУ2 mL3.2ڜuσxϷɢȻ70%3.43 mL2 min4000 r/minx10 minȡŒҺ10 mLɫУό70%3.43 mL2 min…”؏EһΣϲɴҺ50%3.3̶ȣV^Ҫrm50%Һ3.3ϡጣϡҺ0.22 μmVĤ^VVҺyҺ

5.3xl

5.3.1 ɫVl

ɫV C18 150 ×2.0 mm2.2 μmЧɫV

ݶϴÓ

rg/min

VA/%

VB/%

0

95

5

24

15

85

26

15

85

27

95

5

31

95

5

٣0.3 mL/min

أ40

M10 μL

5.3.2 |Vl

늇FxԴESIԴ

Oyģʽ xӡؓxӶxӷOyģʽOyxӌPOҊ2

  2   63NɷֱOyxӌPO

̖

|Q

ĸxӣm/z

m/z

CEV

1

395.2

*357.1

20

 

 

 

225.1

27

2

361.2

*343.1

14

 

 

 

147.4

38

3

359.2

*341.1

14

 

 

 

147.0

35

4

379.1

*359

12

 

 

 

341

16

5

仯ɵ

363.2

*121.0

33

 

 

 

105.1

67

6

ɵ

361.2

*163.1

30

 

 

 

121.0

40

7

׻

375.2

*357.1

15

 

 

 

161.1

29

8

393.2

*355.0

18

 

 

 

146.8

37

9

393.2

*355.0

17

 

 

 

146.8

40

10

411.2

*253.0

25

 

 

 

121.1

47

11

409.2

*279.1

28

 

 

 

147.1

32

12

ε

435.2

*338.9

20

 

 

 

396.9

15

13

ε

417.2

*323.3

17

 

 

 

225.1

30

14

s

435.2

*321.2

20

 

 

 

397.1

16

15

p

453.2

*121

40

 

 

 

337.2

20

16

p

479.2

*440.9

14

 

 

 

321

22

17

s

437.2

*361

26

 

 

 

285.2

30

18

403.2

*147

32

 

 

 

307.1

17

19

377.2

*278.9

20

 

 

 

320.9

16

20

仯ɵɴ

405.2

*309.1

24

 

 

 

120.8

44

21

ɵɴ

423.2

*238.9

39

 

 

 

120.9

41

22

ط

442.2

*141.9

40

 

 

 

123.9

40

23

ɴ

401.2

*295.0

23

 

 

 

146.8

39

24

ɵɴ

403.2

*162.8

37

 

 

 

343

26

25

u

445.1

*154.8

32

 

 

 

287

20

26

׻

417.2

*399.2

12

 

 

 

253.2

25

27

ɴ

435.21

*309

22

 

 

 

337

16

28

289.2

*97.1

35

 

 

 

109

30

29

ɴ

435.2

*309

20

 

 

 

337

19

30

ε

431.2

*413.1

15

 

 

 

146.9

31

31

仯ɵɶ

433.2

*345

19

 

 

 

120.8

31

32

ϩͪ

309.1

*241.1

30

 

 

 

199.2

44

33

419.2

*279

26

 

 

 

321

21

34

ײGͪ

303.2

*108.9

29

 

 

 

97

30

35

仯ɵ

447.3

*345.2

21

 

 

 

120.8

31

36

ε´

477.2

*338.9

22

 

 

 

320.8

25

37

p

495.2

*316.8

23

 

 

 

278.8

27

38

495.2

*120.8

52

 

 

 

337

25

39

ȲZͪ

313.2

*245.3

24

 

 

 

109

33

40

477.3

*354.9

14

 

 

 

278.8

28

41

ε

455.2

*104.9

63

 

 

 

121

38

42

489.2

*380.9

13

 

 

 

114.8

25

43

杊Z

467.2

*359.1

18

 

 

 

265.1

44

44

p

521.2

*301

25

 

 

 

279

24

45

ε

503.2

*338.9

22

 

 

 

321

23

46

u

485.2

*391.2

17

 

 

 

353.1

20

47

ȱ

467.2

*372.9

17

 

 

 

354.9

20

48

濨ɱ

501.2

*312.9

19

 

 

 

292.9

21

49

Īɿ

521.1

*503

13

 

 

 

263

38

50

׵ͪ

385.1

*325.1

20

 

 

 

267.3

24

51

ȵͪ

405.1

*309.3

23

 

 

 

267.3

30

52

p

505.2

*318.9

20

 

 

 

278.9

35

53

Swͪ

315.2

*109

30

 

 

 

97.3

30

54

387.2

*327

18

 

 

 

122.9

35

55

p

521.2

*503

14

 

 

 

319

20

56

p

479.2

*375.3

18

 

 

 

439.4

17

57

ȱɶ

479.2

*342.8

24

 

 

 

278.9

24

58

429.1

*313.2

19

 

 

 

271.3

27

59

541.3

*523.2

18

 

 

 

323.2

25

60

ƶ

271.2

*182.9

-50

 

 

 

145.2

-50

61

287.1

*171

-50

 

 

 

143.2

-60

62

ͪ

269.1

*145

-50

 

 

 

183.1

-50

63

ϩƷ

267.1

*251.2

-35

 

 

 

222.2

-42

      ע“*”鶨xӌ

5.4 

ȡyҺc˜ҺͬlœyƷʬFxӌͶxӌɫV壬yɷֵxӷ屣rgc˜Һırgһ£xĶxӵSȱcஔȘ˜ƷҺĶxӵSȱȵƫ^3ҎtжƷдڌļسɷ֡

עʹ|ؘ˜ʻҺM|ؗlɷ־zxӌSN≥7rgƫ±3%ȡƷЙzԳɷ֕rSĘ˜ҺMд_C

3 жrxSȵSƫ

xSȣk

k>50%

50 %≥ k > 20 %

20 %≥ k>10 %

k≤ 10 %

±20%

±25%

±30%

±50%

5.5 

5.5.1 ˜ʃҺƂ

Qȡyؘ˜Ʒs10mg_0.00001 g100 mLƿУ棨3.1ʹܽⲢ̶ȡ

5.5.2ϵл|˜ҺƂ

ȡcyƷ|ͬհטƷ610 mLɫУ0.2 g/ݣքe˜ʃҺm“5.2Ʒ̎IJE̎Ȼ50%Һ3.3ϵл|˜Һзsɡuɡε¡ƶͪȞ61020304060 ng/mLM֝Ȟ 2410204060 ng/mL˜ҺȷɸHrM{

5.5.3 Ʒ̎ͬ5.2

5.5.4 y

ȡϵл|˜ҺMӣӛ䛶xӌɫVeLƷeA-ȣC˜侀Pϵr≥0.99ȡyҺMӣyöxɫVe˜õyҺиɷֵĝȣ“6”ӋƷиɷֵĺ

6

6.1Ӌ

 

ʽУω——ƷмMֵ|֔µg/g

ρ——Ę˜õyMֵ|ȣµg/mL

V——ƷwemL

m——Ʒȡg

D——ϡጱδϡጄt1

؏ԗl«@õăɴΪyԇYĽ^ֵó^gƽֵ15 %

6.2 ʺ;ܶ

ҌCޝȻʞ72.7122.1%˜ƫС15%n=6Ȼʞ80.7119.6%˜ƫС11%n=6


A

YԸ䛣

63NصQӢQCAS̖ʽ

̖

Q

ӢQ

CAS̖

ʽ

1

Triamcinolone

124-94-7

C21H27FO6

2

Prednisolone

50-24-8

C21H28O5

3

Prednisone

53-03-2

C21H26O5

4

9-fluoroprednisolone

338-95-4

C21H27FO5

5

仯ɵ

Hydrocortisone

50-23-7

C21H30O5

6

ɵ

Cortisone

53-06-5

C21H28O5

7

׻

Methylprednisolone

83-43-2

C22H30O5

8

Betamethasone

378-44-9

C22H29FO5

9

Dexamethasone

50-02-2

C22H29FO5

10

Flumethasone

2135-17-3

C22H28F2O5

11

Beclomethasone

4419-39-0

C22H29ClO5

12

ε

Triamcinolone acetonide

76-25-5

C24H31FO6

13

ε

Desonide

638-94-8

C24H32O6

14

s

Flunisolide

77326-96-6

C24H31FO6

15

p

Fluocinolone acetonide

67-73-2

C24H30F2O6

16

p

Triamcinolone diacetate

67-78-7

C25H31FO8

17

s

Fludroxycortide

1524-88-5

C24H33FO6

18

Prednisolone 21-acetate

52-21-1

C23H30O6

19

Fluorometholone

426-13-1

C22H29FO4

20

仯ɵɴ

Hydrocortisone 21-acetate

50-03-3

C23H32O6

21

ɵɴ

Fludrocortisone 21-acetate

514-36-3

C23H31FO6

22

ط

Deflazacort

14484-47-0

C23H29NO4

23

ɴ

Prednisone 21-acetate

125-10-0

C23H28O6

24

ɵɴ

Cortisone 21-acetate

50-04-4

C23H30O6

25

u

Halometasone

50629-82-8

C22H27ClF2O5

26

׻

Methylprednisolone 21-acetate

53-36-1

C24H32O6

27

ɴ

Betamethasone 21-acetate

987-24-6

C24H31FO6

28

Testosterone

58-22-0

C19H28O2

29

ɴ

Dexamethasone 21-acetate

1177-87-3

C24H31FO6

30

ε

Budesonide

51333-22-3

C25H34O6

31

仯ɵɶ

Hydrocortisone 17-butyrate

13609-67-1

C25H36O6

32

ϩͪ

Gestrinone

16320-04-0

C21H24O2

33

Fluorometholone 17-acetate

3801-06-7

C24H31FO5