Methods for impurity profiling of heroin and cocaine

64

Methods for impurity profiling of heroin and cocaine

Figure II.

lectropherogram of a standard mixture of heroin, 

O

6

-monoacetylmorphine, O

3

-monoacetylmorphine, morphine, acetylcodeine, 

papaverine, codeine and noscapine

Conditions: A 64-cm (55.5 cm to detector window) x 50-µm i.d. fused silica capillary oper-

ating at 25° C and 30 kV with UV detection at 205 nm was used. Pressure injections of

500 mbar*s were used with a run buffer consisting of Celixir reagent B (pH 2.5) + 100 mM

DM-ß-CD. For migration times, see table 1.

Source: Reprinted from Journal of Chromatography A, vol. 1034, Nos. 1-2, I. S. Lurie and others,

“Use of dynamically coated capillaries for the determination of heroin, basic impurities and adulter-

ants with capillary electrophoresis”, pp. 227-235, Copyright 2004, with permission from Elsevier.

Peaks:

a = heroin (0.40 mg/ml)

b = O

6

-monoacetylmorphine (0.09 mg/ml)

c = O

3

-monoacetylmorphine (0.04 mg/ml)

d = morphine (0.04 mg/ml)

e = acetylcodeine (0.04 mg/ml)

f = papaverine (0.04 mg/ml)

g = codeine (0.04 mg/ml)

h = noscapine (0.06 mg/ml)

---

Annex III

65

Table 1.

Relative migration times of heroin, basic impurities and 

basic adulterants for the electropherogram in figure II

Solute

Relative

a

migration time (min)

Thiamine

0.562

Nicotinamide

0.666

D- or L- Chloroquine

0.713

D- or L- Chloroquine

0.717

Quinine

0.815

Quinine impurity

0.856

Heroin

0.927

O

6

-monoacetylmorphine

0.953

Dipyrone

0.957

O

3

-monoacetylmorphine

0.965

Aminopyrene

0.968

Lidocaine

0.968

Morphine

0.983

Acetylcodeine

1.00 (12.4)

Papaverine

1.02

Strychnine

1.03

Codeine

1.05

L-Ephedrine

1.07

L-Pseudoephedrine

1.07

D-Ephedrine

1.08

Xylazine

1.10

D-Pseudoephedrine

1.10

Noscapine

1.11

Thebaine

1.12

Procaine

1.14

Chlorpheniramine

1.15

Brompheniramine

1.16

Cocaine

1.22

trans-Doxepin

1.23

Diphenhydramine

1.23

Tetracaine

1.23

cis-Doxepin

1.24

t

0

1.85

Source: Reprinted from Journal of Chromatography A, vol. 1034, Nos. 1-2, I. S. Lurie and others,

“Use of dynamically coated capillaries for the determination of heroin, basic impurities and adulter-

ants with capillary electrophoresis”, pp. 227-235, Copyright 2004, with permission from Elsevier.

a

Relative to acetylcodeine. 

---

66

Methods for impurity profiling of heroin and cocaine

Figure III.

Electropherogram of a standard mixture of acetaminophen, 

theophylline, caffeine, aspirin, salicylic acid, antipyrene, phenobarbitol 

and phenacetin

Conditions: A 32-cm (23.5 cm to detector window) x 50-µm i.d. fused silica capillary oper-

ating at 15° C and 8.5 kV with UV detection at 195 nm was used. Pressure injections of

100 mbar*s were used with a run buffer consisting of 50 mM phosphate-borate (pH 6.5)

+ 103.2 mM (3%, w/w) SDS: For migration times, see table 2. 

Source: Reprinted from Journal of Chromatography A, vol. 1034, Nos. 1-2, I. S. Lurie and others,

“Use of dynamically coated capillaries for the determination of heroin, basic impurities and adulter-

ants with capillary electrophoresis”, pp. 227-235, Copyright 2004, with permission from Elsevier.

Peaks:

a = acetaminophen (0.08 mg/ml)

b = theophylline (0.09 mg/ml

c = caffeine (0.09 mg/ml)

d = aspirin (0.09 mg/ml)

e = salicylic acid (0.09 mg/ml)

f = antipyrene (0.10 mg/ml)

g = phenobarbital (0.10 mg/ml)

h = phenacetin (0.10 mg/ml)

---

Annex III

67

Table 2.

Relative migration times of acidic and neutral adulterants, 

basic impurities and basic adulterants for the electropherogram in figure III

Solute

Relative migration time (min)

t

0

0.504

Nicotinamide

0.591

Acetominophen

0.660

Theophylline

0.673

Dipyrone (1)

0.738

Caffeine

0.764

Aspirin

0.809

Salicylic acid

0.860

Anitipyrene

0.948

Phenobarbital

1.00 (6.8)

Ibuprofen

1.11

Aminopyrene

1.11

Phenacetin

1.13

Dipyrone (2)

1.13

Benzocaine

1.25

Thiamine

1.32

Morphine

1.35

Codeine

1.44

O

3

-monoacetylmorphine

1.44

Procaine

1.45

Pseudoephedrine

1.45

Ephedrine

1.45

Lidocaine

1.46

Heroin

1.47

O

6

-monoacetylmorphine

1.47

Acetylcodeine

1.47

Noscapine

1.47

Quinine

1.48

Chloroquine

1.48

Yohimbine

1.48

Strychnine

1.48

Thebaine

1.48

Xylazine

1.49

Cocaine

1.49

Tetracaine

1.49

cis- and trans-Doxepin

1.50

Brompheniramine

1.50

Methorphan

1.50

Papaverine

1.50

Chlorpheniramine

1.51

Diphenhydramine

1.51

Source: Reprinted from Journal of Chromatography A, vol. 1034, Nos. 1-2, I. S. Lurie and others,

“Use of dynamically coated capillaries for the determination of heroin, basic impurities and adulter-

ants with capillary electrophoresis”, pp. 227-235, Copyright 2004, with permission from Elsevier.

---