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. 2022 Sep 21;14(10):2003. doi: 10.3390/pharmaceutics14102003

Table 9.

Overview of thermal characterization (DSC) of amorphous samples obtained by ball milling.

# Sample Molar Ratio/Composition Glass Transition Temperature (Tg)/(°C) Milling Temperature Conditions Ref.
2A Furosemide-arginine 1:1 127 ± 0.5 5 °C 2 °C/min, −10 °C to 180 °C, 50 mL/min [85]
Furosemide-citrulline 1:1 77.1 ± 5.6
Nitrofurantoin-arginine 1:1 139.1 ± 0.2
Nitrofurantoin-citrulline 1:1 49.3 ± 2.1/108.5 ± 0.3
Cimetidine-arginine 1:1 40.4 ± 3.1
Cimetidine-citrulline 1:1 39.5 ± 1.5
Mebendazole-arginine 1:1 53.5 ± 3.3/112.2 ± 0.4
Mebendazole-citrulline 1:1 43.6 ± 1.2/112.1 ± 0.2
3A Sulfathiazole-polyvinylpyrrolidone STZ/PVP Xpvp = 0.4 173.2 Room temperature 10 °C/min [86]
Sulfadimidine-polyvinylpyrrolidone SDM/PVP Xpvp = 0.6 146.7
4A Naproxen-cimetidine 1:1 34.5 4 ± 2 °C 10 K min−1 [87]
2:1 31.5
1:2 40.2
5A γ-indomethacin–ranitidine hydrochloride 1:1 32.5 4 ± 2 °C 10 K per min from 0 to 160 °C [28]
2:1 34.3
1:2 29.3
6A γ-indomethacin N/A 39.23 4 ± 2 °C 10 K min−1 from 0 to 180 °C under nitrogen gas flow 50 mL min−1 [88]
α-indomethacin N/A 37.92
7A Tadafil N/A 147 Cryogenic temperature (liquid nitrogen) 10 °C/min under nitrogen atmosphere (60 mL/min) [26]
8A Glibenclamide N/A 65 Cryogenic temperature (samples immersed in liquid nitrogen) 10 K/min from 20 to 190 °C [89]
9A Trehalose dihydrate N/A 21 Cryogenic temperature (samples immersed in liquid nitrogen) 10 °C/min from 0 to 150 °C [90]
10A Atenolol-hydrochlorothiazide 1:1 311.44 Cryogenic temperature (samples immersed in liquid nitrogen) 10 °C/min, starting at −20 °C [91]
1:2 315.82
2:1 Not determined due to fast recrystallization
11A Indomethacin-tryptophan 1:1 Tg ranges from 120 to 45 °C, decreasing as mol% of Ind increases 6 °C 2 K/min from −20 to 180 °C [92]
Furosemide-tryptophan 1:1 Tg ranges from 138 to 80 °C, decreasing as mol% of Fur increases
12A Dexamethasone N/A 115 < Tg < 120 Room temperature 0.663 °C and 50 S, “Heat only” conditions [27]
13A α-lactose N/A 70 30 ± 5% relative humidity and 22 ± 3 °C From 0 to 240°, 10 °C/min under N2 flow of 50 mL/min [93]
14A α-D-glucose N/A 38 −15 °C and 0% relative humidity 5 °C/min, flushed with highly pure nitrogen gas [68]
15A Mebendazole-ASPA 1:1 91 5 °C, cold room −10 °C to 180 °C, 2 °C/min, nitrogen flow was 50 mL/min [94]
Tadalafil-ASPA 1:1 102.9
Piroxicam-ASPA 1:1 76
16A α-D-glucose N/A 38 −15 °C and 0% relative humidity 5 °C/min [95]
β-D-glucose N/A 39 5 °C/min
17A Carvedilol, carbamazepine, furosemide, indomethacin, mebendazole-amino acids 1:1 A single Tg for each formulation Cold room (+6 °C) Nitrogen flow of 50 mL/min, 2 °C/min
heated to 180 °C
[31]
18A Indomethacin-lysine 1:1 100 (DMB) Cold room (+6 °C) Nitrogen flow of 50 mL/min, 2 °C/min
heated to 180 °C
[96]
19A Mebendazole-tryptophan Xmeb = 0.1 53.5 Room temperature −5 °C to 210 °C at 10 °C/min [97]
Pioglitazona-tryptophan Xpgz = 0.1, 150 min 44.9
22A (S)-naproxen-L-arginine 1:1 91.9 ± 0.2 6 °C Nitrogen flow of 50 mL/min, 2 °C/min from −10 °C to 180 °C [99]
23A Griseofulvin-tryptophan 1:1 113.46 NR 25 to 300 °C, 5 °C/min [100]
24A Naproxen-tryptophan-proline 1:1:1 55.1 ± 3.1 6 °C Nitrogen flow of 20 mL/min, 10 K/min, from −20 to 170 °C [101]
Naproxen-tryptophan 1:1 58.2 ± 0.5
Tryptophan-proline 1:1 67.2 ± 6.8
25A Mebendazole-tryptophanphenylalanine 1:1:1 107.5 ± 0.2 5 °C 2 °C/min, heating to 180 °C [102]
Mebendazole-phenylalaninetryptophan 1:1:1 104.6 ± 0.2
Mebendazole-aspartatetyrosine 1:1:1 61.2 ± 0.9
Mebendazole-histidineglycine 1:1:1 34.9 ± 1.2/89 ± 0.6
Mebendazole-prolinetryptophan 1:1:1 6.5 ± 0.2
Mebendazole-tryptophan 1:1 128.7 ± 0.2
Mebendazole-proline 1:1 96.9 ± 0.1
Mebendazole-proline-tryptophan 1:1:1 56.3 ± 0.2
Mebendazole-tryptophan-phenylalanine 1:1:1 119 ± 0.1
27A Indomethacin-arginine 1:1 117 ± 4 6 °C Nitrogen gas flow of 50 mL/min, 2 °C/min, from −10 to 180 °C, 0.212 °C and a period of 40 s [104]
29A Naproxen-NAP(Na) 2:1 55.8 4 °C 2 °C/min,
0.2120 °C with a period of 40 s
[106]
1:1 40
1:2 NR
31A Indomethacin-arginine 1:1 62.9 ± 0.8 NR Nitrogen gas flow of 50 mL/min, 10 °C/min to 180 °C [36]
Indomethacin-phenylalanine 55.3 ± 0.4
Indomethacin-tryptophan 62.7 ± 7.0
32A Simvastatin-lysine 1:1 33.2 ± 0.9 6”C Nitrogen flow of 50 mL/min, 10 °C/min, from −50 °C to 280 °C (depending on the sample) [108]
Glibenclamide-serine 1:1 70.1 ± 1.3
Glibenclamide-threonine 1:1 58.4 ± 1.3
Glibenclamide-serine-threonine 1:1:1 62.5 ± 4.5
33A Indomethacin-arginine 1:1 36.7 ± 0.8 6 °C Nitrogen gas flow, 20 mL/min, from −20 to 180 °C, 10 K/min [98]
Indomethacin-phenylalanine 1:1 64.1 ± 1.4
Indomethacin-tryptophan 1:1 47.8 ± 2.9
Indomethacin-phenylalanine-tryptophan 1:1:1 68.7 ± 2.6
Indomethacin-arginine-phenylalanine 1:1:1 63.1 ± 0.8
Carbamazepine-tryptophan 1:1 81 ± 0.6 Nitrogen gas flow, 20 mL/min, from −20 to 200 °C, 10 K/min
Carbamazepine-phenylalanine-tryptophan 1:1:1 75.1 ± 1.1
Carbamazepine-arginine-tryptophan 1:1:1 65.4 ± 1.1
35A Carbamazepine-citric acid 1:1 38.8 ± 2.7 4 °C Nitrogen gas at 50 mL/min, 2 °C/min from 0 to 150 °C, 0.212 °C with a period of 40 s [110]
Citric acid-arginine 1:1 56.2 ± 0.7
Citric acid-arginine 1:2 106 ± 0.3
Citric acid-arginine 1:3 130.5 ± 0.1
Citric acid-arginine 1:4 119 ± 0.1
Carbamazepine-citric acid-arginine 1:1:1 77.8 ± 1.8
Carbamazepine-citric acid-arginine 1:1:2 105.3 ± 0.2
Carbamazepine-citric acid-arginine 1:1:3 127.8 ± 0.8
36A Glibenclamide-quercetin 1:1 85.97 ± 0.29 Cryomilled Nitrogen glow of 50 mL/min, 1 °C/min [111]
37A Mebendazole-glutamate-arginine (crystalline salt) 1:1:1 37.8 Cold rooms (5 °C) Nitrogen gas flow of 50 mL/min, 2 °C/min, 0.212 °C (amplitude), 40 s (period) [112]
Mebendazole-glutamate-arginine (amorphous salt) 1:1:1 37.3
Meb-glutamatearginine 1:1 36.5/77
Meb-arginineglutamate 1:1 36.3/76.3
42A Candesartan cilexetil-hydrochlorothiazide NA 110 Room temperature Nitrogen gas flow, 100 mL/min, 10 °C/min, from 30 to 300 °C [116]