Table 2.
Batch‐to‐batch analysis of the NF
| Parameter | Method of analysis | Batch number | |||
|---|---|---|---|---|---|
| #1 | #2 | #3 | #4 | ||
| Appearance | Visual | White | White | White | White |
| Identity | Infrared spectrometry | Corresponds to specifications | Corresponds to specifications | Corresponds to specifications | Corresponds to specifications |
| Calcidiolj 25(OH)D3.H2O | HPLC/UVa | 100.6% | 101.3% | 101.1% | 102.2% |
| ∆22‐25(OH)D3 | HPLC/UV | 0.2% | 0.2% | 0.3% | 0.2% |
| 25(OH) lumisterol(f) | HPLC‐MSc | 0.14% | 0.14% | 0.1% | 0.1% |
| pre‐25(OH)D3 (g) | HPLC‐MS | 0.14% | 0.14% | 0.1% | 0.1% |
| iso‐25(OH) Tachysterol(h) | HPLC‐MS | 0.14% | 0.14% | 0.1% | 0.1% |
| trans‐Vitamin D3 (i) | HPLC‐MS | 0.14% | 0.14% | 0.1% | 0.1% |
| Other impurities | HPLC‐MS | 0.09% | 0.09% | 0.10% | 0.10% |
| Water content | Karl Fisher | 4.4% | 4.4% | 4.9% | 4.5% |
| Acetone mg/kg | GC‐HS‐FIDd | 840 | 821 | 789 | 840 |
| Isopropanol mg/kg | GC‐HS‐FID | NDb | NDb | NDb | NDb |
| Heavy metals | |||||
| Arsenic mg/kg | ICP‐MSe | < 1.0 | < 1.0 | < 1.0 | < 1.0 |
| Lead mg/kg | ICP‐MS | < 1.0 | < 1.0 | < 1.0 | < 1.0 |
| Mercury mg/kg | ICP‐MS | < 0.1 | < 0.1 | < 0.1 | < 0.1 |
| Cadmium mg/kg | ICP‐MS | < 0.5 | < 0.5 | < 0.5 | < 0.5 |
a
HPLC/UV: High performance liquid chromatography/Ultraviolet Spectroscopy.
b
ND: Not Detectable.
c
HPLC–MS: High‐performance liquid chromatography/mass spectrometry.
d
GC‐HS‐FID: Gas Chromatography with Headspace‐Sampler and Flame Ionisation Detector.
e
ICP‐MS: Inductively coupled plasma/mass spectrometry.
f
Impurity: 9β,10α‐cholesta‐5,7‐diene‐3β,25‐diol.
g
Impurity: Cholesta‐5,7‐diene‐3β,25‐ diol.
h
Impurity: (6E)‐9,10‐secocholesta‐5(10),6,8‐triene‐3β,25‐diol (iso‐ 25(OH).
i
Impurity: (5E,7E)‐9,10‐secocholesta‐5,7,10(19)‐triene‐3β,25‐diol.
j
Values exceeding 100% are due to technical variabilities.