AOAC CASP SMPRs

Table 1. Residual solvents and targeted LOQs

Table 1. ( continued )

Analytical range Lower (≤ ppm) Upper (ppm)

Analytical range Lower (≤ ppm) Upper (ppm)

Proposed target LOQ, ppm

Proposed target LOQ, ppm

Residual solvents a

Residual solvents a

Class 1

Ethyl acetate

5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000

2500 2500 2500 2500 2500 2500 2500 2500 2500 2500 2500 2500 2500 2500 2500 2500

150000 150000 150000 150000 150000 150000 150000 150000 150000 150000 150000 150000 150000 150000 150000 150000

Benzene

2 4 5 8

1 2

60

Ethyl ether

Carbon tetrachloride 1,2-Dichloroethane 1,1-Dichloroethene 1,1,1-Trichloroethane

120 150 240

Ethyl formate Formic acid

2.5

4

Heptane

1500

750

45000

Isobutyl acetate Isopropyl acetate Methyl acetate 3-Methyl-1-butanol Methylethylketone Methylisobutylketone 2-Methyl-1-propanol

Class 2

Acetonitrile

6

3

180

Chlorobenzene

360

180

10800

Chloroform

60 70

30 35

1800 2100

Cumene

Cyclohexane

3880 1870

1940

116400 56100

1,2-Dichloroethene 1,2-Dimethoxyethane N,N -dimethylacetamide N,N -dimethylformamide

935

Pentane

100

50

3000

1-Pentanol 1-Propanol 2-Propanol

1090

545 440 190 310 110 145 80

32700 26400 11400

880 380 160 620 220 290

1,4-Dioxane

Isopropanol (2-propanol) Propyl acetate

2-Ethoxyethanol Ethylene glycol

4800

5000

2500

150000

18600

Additional

Formamide

6600 8700

Butane (sum of n - and iso-)

5000

2500

150000

Hexane

Propane

12

6

360

n -Hexane Methanol

2,2-Dimethylbutane 2,3-Dimethylbutane

290 290

145 145

8700 8700

400

200

12000

2-Methoxyethanol Methylbutylketone Methylcyclohexane Methylene chloride N -Methylpyrrolidone

50 50

25 25

1500 1500

2-Butanone

5000 5000

2500 2500

150000 150000

2-Methylbutane 2-Methylpentane 3-Methylpentane Ethylbenzene Ethylene oxide

1180

590 300 265

35400 18000 15900

290 290

145 145

8700 8700

600 530

2170

1085

65100

Nitromethane

50

25

1500 6000 4800

50 12 12

25

1500

Pyridine Sulfolane

200 160 720 100

100

Isobutane (methyl propane)

6 6

360 360

80

n -Butane n -Heptane n -Pentane Nitrogen o -Xylene

Tetrahydrofuran

360

21600

1000 1000

500 500

30000 30000

Tetralin Toluene

50 15 40

3000

30 80

900

0

0 5

Trichloroethylene

2400

10

300

Xylene

2170

1085

65100

Triethylamine

5000

2500

150000

m,p -Xylenes

a  USP Guidance (467) Residual Solvents.

Class 3

Acetic acid Acetone Anisole 1-Butanol 2-Butanol Butyl acetate

5000 1000 5000 5000 5000 5000 5000 5000 1000

2500

150000 30000 150000 150000 150000 150000 150000 150000 30000

500

2500 2500 2500 2500 2500 2500

Table 2. Method performance requirements for residual solvents in Table 1

Analytical range, ppm

Parameter

1–100

100–500 90–107

500–1000

>1000 97–103

tert -Butylmethyl ether Dimethyl sulfoxide

Recovery, % 60–120

95–105

RSD r RSD

, %

≤20 ≤30

≤5 ≤8

≤4 ≤6

≤3 ≤4

Ethanol

500

, %

R

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