Comparative study of Mg/Al- and Zn/Al-layered double hydroxide-perindopril erbumine nanocomposites for inhibition of angiotensin-converting enzyme

Figures & data

Figure 1 Powder X-ray diffraction patterns for the nanocomposite, PMAE (A). Inset shows the X-ray diffraction patterns for the nanocomposites PZAE (B) and PZAC (C).²¹

Abbreviations: PMAE, perindopril intercalated into Mg/Al by ion-exchange; PZAE, perindopril intercalated into Zn/Al by ion-exchange; PZAC, perindopril intercalated into Zn/Al by coprecipitation method.

Table 1 XRD data of diffraction peaks and the lattice parameters of PMAE, PZAE and PZAC nanocomposites

Samples	d003 (Å)	d006 (Å)	d009 (Å)	d110 (Å)	a (Å)	c (Å)	M^2+/Al^3+	x	Empirical formula
PMAE	22.83	10.20	6.90	1.51	3.02	64.00	2.04	0.33	[Mg0.67AI0.33(OH)2](PE^−)0.21(NO3^−)0.12·1.4H2O
PZAE*	21.70	10.60	7.08	1.53	3.07	65.60	3.48	0.22	[Zn0.78AI0.22(OH)2](PE^−)0.19(NO3^−)0.03·0.4H2O
PZAC*	19.90	9.96	6.67	1.54	3.07	59.80	2.60	0.28	[Zn0.72AI0.28(OH)2](PE^−)0.177 (NO3^−)0.103·0.91H2O

Note:

* Data from reference.²¹

Abbreviations: Mg, magnesium; Al, aluminum; Zn, zinc; NO₃, nitrate; PE, perindopril erbumine; OH, hydroxide; PMAE, perindopril intercalated into Mg/Al by ion-exchange; PZAE, perindopril intercalated into Zn/Al by ion-exchange; PZAC, perindopril intercalated into Zn/Al by coprecipitation method.

Figure 2 Three-dimension structure of perindopril erbumine (A) and molecular structural models of perindopril intercalated between interlayers of Mg/Al-LDH (B).

Abbreviations: Mg, magnesium; Al, aluminum; LDH, layered double hydroxide.

Figure 3 Fourier transform infrared spectra of perindopril erbumine (A) and PMAE nanocomposite (B). Inset shows the Fourier transform infrared spectra of the nanocomposites PZAE (C) and PZAC (D).²¹

Abbreviations: PMAE, perindopril intercalated into Mg/Al by ion-exchange; PZAE, perindopril intercalated into Zn/Al by ion-exchange; PZAC, perindopril intercalated into Zn/Al by coprecipitation method.

Figure 4 Thermogravimetric and differential thermogravimetric analysis of perindopril (A) and PMAE nanocomposite (B).

Abbreviation: PMAE, perindopril intercalated into Mg/Al by ion-exchange.

Table 2 Shows the weight loss percentages for the three types of the nanocomposites; PMAE, PZAE and PZAC

Samples	First weight loss (%)			Second weight loss (%)			Third weight loss (%)			Last weight loss (%)			Total weight loss (%)
	Onset (°C)	Offset (°C)	Wt loss (%)	Onset (°C)	Offset (°C)	Wt loss (%)	Onset (°C)	Offset (°C)	Wt loss (%)	Onset (°C)	Offset (°C)	Wt loss (%)
PMAE	28	188	10.0	188	278	5.2	280	562	43.2	562	725	3.5	61.9
PZAE*	34	118	4.2	119	258	13.6	257	487	31.1	591	858	7.0	55.9
PZAC*	38	137	6.2	136	244	8.7	246	499	31.8	559	927	12.6	59.3

Note:

* Data from reference.²¹

Abbreviations: PMAE, perindopril intercalated into Mg/Al by ion-exchange; PZAE, perindopril intercalated into Zn/Al by ion-exchange; PZAC, perindopril intercalated into Zn/Al by coprecipitation method.

Table 3 Surface properties for the nanomaterials

Samples	BET surface area (m^2/g)	BJH pore volume (cm^3/g)	BJH pore diameter (Å)
Mg/Al-LDH	3	0.010	108
PMAE	11	0.020	40
Zn/Al-LDH*	1	0.008	243
PZAE*	2	0.009	135
PZAC*	7	0.025	157

Note:

* Data from reference.²¹

Abbreviations: Zn, zinc; Al, aluminum; Mg, magnesium; LDH, layered double hydroxide; PMAE, perindopril intercalated into Mg/Al by ion-exchange; PZAE, perindopril intercalated into Zn/Al by ion-exchange; PZAC, perindopril intercalated into Zn/AI by coprecipitation method; BJH, Barret-Joyner-Halenda; BET, Brunauer-Emmett-Teller.

Figure 5 Adsorption-desorption isotherms (A) and Barret-Joyner-Halenda pore size distributions (B) for Mg/Al-LDH and its nanocomposite with perindopril erbumine, PMAE. Inset in (A) shows the adsorption-desorption isotherms for PZAE, PZAC, and ZnAl-LDH.²¹

Abbreviations: Mg, magnesium; Al, aluminum; LDH, layered double hydroxide; PMAE, perindopril intercalated into Mg/Al by ion-exchange; PZAE, perindopril intercalated into Zn/Al by ion-exchange; PZAC, perindopril intercalated into Zn/Al by coprecipitation method; Zn, zinc; STP, standard temperature pressure.

Figure 6 Field emission scanning electron microscopic images of Mg/Al-LDH (A–C) and PMAE (D–F).

Abbreviations: PMAE, perindopril intercalated into Mg/Al by ion-exchange; Mg, magnesium; Al, aluminum; LDH, layered double hydroxide.

Figure 7 (I) Release profiles of perindopril from the PMAE nanocomposite at pH 4.8 (C) and pH 7.4 (D) up to 1500 minutes, (II) release profiles of perindopril up to 5000 minutes at pH 7.4. Inset shows the release profiles of perindopril from its physical mixture of perindopril with Mg/Al-LDH at pH 4.8 (A) and pH 7.4 (B).

Abbreviations: PMAE, perindopril intercalated into Mg/Al by ion-exchange; Mg, magnesium; Al, aluminum; LDH, layered double hydroxide.

Table 4 Correlation coefficient (R²), rate constants (K) and half time (t_1/2) obtained by fitting the perindopril release data from PMAE nanocomposite into solutions at pH 4.8 and 7.4

pH	Saturation release (%)	R^2			Pseudo-second order
		Pseudo-first order	Parabolic diffusion model	Pseudo-second order	Rate constant, K (mg/min) × 10^−5	t1/2 (min)
7.4	100	0.7739	0.7006	0.9901	3.17	315
4.8	100	0.9651	0.9190	0.9953	6.30	145

Abbreviation: PMAE, perindopril intercalated into Mg/Al by ion-exchange.

Figure 8 Fitting the data of perindopril release from PMAE at 7.4 (A–C) and at 4.8 (D–F).

Abbreviation: PMAE, perindopril intercalated into Mg/Al by ion-exchange.

Figure 9 MTT assays of normal Chang liver cells after 24 hours of treatment with perindopril erbumine, PMAE, and Mg/Al-LDH.

Abbreviations: PMAE, perindopril intercalated into Mg/Al by ion-exchange; Mg, magnesium; Al, aluminum; LDH, layered double hydroxide.

Table 5 ACE activity for perindopril erbumine, PMAE, PZAE, PZAC and Mg/Al-LDH at different exposure times

Exposure time (minutes)	Perindopril erbumine	PMAE	MgAl-LDH	PZAE*	PZAC*
30	90.8	56.6	−0.8	43.4	21.5
60	93.6	58.3	1.80	68.2	55.2
90	97.3	70.6	5.60	70.1	55.4

Note:

* Data obtained from reference.²¹

Abbreviations: ACE, Angiotensin-converting enzyme; Mg, magnesium; Al, aluminum; LDH, layered double hydroxide; PMAE, perindopril intercalated into Mg/Al by ion-exchange; PZAE, perindopril intercalated into Zn/Al by ion-exchange; PZAC, perindopril intercalated into Zn/AI by coprecipitation method.

Figure 10 ACE inhibition (%) for free perindopril and intercalated perindopril, PMAE, PZAE, PZAC, and Mg/Al-LDH at exposure times of 30, 60, and 90 minutes.

Abbreviations: Mg, magnesium; Al, aluminum; LDH, layered double hydroxide; PMAE, perindopril intercalated into Mg/Al by ion-exchange; PZAE, perindopril intercalated into Zn/Al by ion-exchange; PZAC, perindopril intercalated into Zn/Al by coprecipitation method; Zn, zinc.

Al AliSHHAl-QubaisiMHusseinMZIsmailMZainalZHakimMNControlled release and angiotensin-converting enzyme inhibitor properties of an antihypertensive drug based on a perindopril erbumine-layered double hydroxide nanocompositeInt J Nanomedicine201272129214122619549

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