cyclolab

C42H70-nO35 · (C4H8O3SNa)n

1135.0 + n·(158.2)

4-Hydroxybutane-1-sulfonic acid sodium salt, bis(4-sulfobutyl) ether disodium, residual beta-cyclodextrin

Water: > 50 g
Methanol: < 0.5 g
Acetone: < 0.5 g

Appearance

Visual

white or off-white powder

Identification A

IR (USP <197>, EP 2.2.24)

complies with SBECD reference

Identification B

HPLC (USP <621>, EP 2.2.29)

tR of major peak complies with SBECD reference

Identification C

CE (USP <1053>, EP 2.2.47)

Average Degree of Substitution: 6.2 - 6.9

Identification D

Sodium ID (USP <191>, EP 2.3.1)

positive test

Assay

HPLC (USP <621>, EP 2.2.29)

95.0 - 105.0% on the anhydrous basis

Heavy metals

ICP-MS (USP <232, 233>

Cadmium  NMT 0.5 µg/g
Lead  NMT 0.5 µg/g
Arsenic  NMT 1.5 µg/g
Mercury  NMT 3.0 µg/g
Chromium  NMT 110 µg/g
Nickel  NMT 2 µg/g
Molybdenium  NMT 150 µg/g
Vanadium  NMT 1 µg/g

Limit of related substances
beta-cyclodextrin (Betadex)
total other impurities

HPLC (USP <621>, EP 2.2.29)

NMT 0.1%
NMT 1.0%

Limit of 1,4-Butane Sultone

GC (USP <621>, EP 2.2.28)

NMT 0.5 ppm

Limit of Sodium Chloride

Limit test (USP <221>)

NMT 0.2%

Limit of 4-Hydroxybutane-1-sulfonic Acid

CE (USP <1053>, EP 2.2.47)

NMT 0.09%

Limit of Bis(4-sulfobutyl) Ether Disodium

CE (USP <1053>, EP 2.2.47)

NMT 0.05%

Bacterial Endotoxin Test

EP-USP harmonized method

≤ 24 IU/g

Microbial Enumeration Tests

EP-USP harmonized method

TAMC ≤ 100 cfu/g
TYMC ≤ 50 cfu/g

Test for Specified Microorganism

EP-USP harmonized method

absence of Escherichia Coli /1 g

Phosphate content

UV-Vis Spectroscopy (USP <851>, EP 2.2.25)

525-700 μg/g

Clarity of solution (30%, w/v)

Visual, see details in the USP Monograph, EP 2.2.1

the solution is clear, and essentially free from particles of foreign matter

Average Degree of Substitution (n)

CE (USP <1053>, EP 2.2.47)

6.2 - 6.9

Peak distribution

CE (USP <1053>, EP 2.2.47)

each SBECD peak (I-X) meets the limit range (peak area %) of the Monograph

SBECD sodium                  Limit range
peaks                                (% peak area)

I (DS-1)                                 0 - 0.3
II (DS-2)                                0 - 0.9
III (DS-3)                               0.5 - 5.0
IV (DS-4)                              2.0 - 10.0
V (DS-5)                               10.0 - 20.0
VI (DS-6)                              15.0 - 25.0
VII (DS-7)                             20.0 - 30.0
VII (DS-8)                             10.0 - 25.0
IX (DS-9)                              2.0 - 12.0
X (DS-10)                             0 - 4.0

Residual solvents: ethanol

GC (USP <621>, EP 2.2.28)

NMT 2500 ppm

pH (30%, w/V)

USP <791>

4.0 - 6.8

Water content

USP <921> Method I, EP 2.5.12

NMT 10.0 %