Gold nanoparticle-enhanced luminol/ferricyanide chemiluminescence system for aristolochic acid-I detection in medicinal plants and slimming products

Figures & data

Figure 1. Chemical structure of aristolochic-I sodium salt.

Figure 2. (a) TEM image of AuNPs and (b) UV-absorption spectrum of AuNPs.

Figure 3. Selection of suitable oxidizing agents for CL reaction.

Figure 4. Effect of luminol and potassium ferricyanide concentration on CL intensity, for luminol concentration (1.5 mL of AuNPs solution and potassium ferricyanide 1.0 × 10⁻² mol L⁻¹) and for potassium ferricyanide concentration (1.5 mL of prepared AuNPs and luminol 2.0 × 10⁻⁴ mol L⁻¹) with AA-I 25 g mL⁻¹.

Figure 5. Effect of added volume of AuNPs on SIA-CL luminol-potassium ferricyanide system.

Figure 6. Effect of sodium hydroxide, ammonium hydroxide, sodium carbonate and sodium bicarbonate concentration on CL intensity of luminol-potassium ferricyanide system (1.5 mL of AuNPs, potassium ferricyanide 1.0 × 10⁻² mol L⁻¹ and luminol 2.0 × 10⁻⁴ mol L⁻¹).

Figure 7. The influence of flow rate on the relative CL intensity. Conditions; 50 µL of 2.0 × 10⁻⁴ mol L⁻¹ luminol; 30 µL of AuNPs and 30 µL of 1.0 × 10⁻² mol L⁻¹ potassium ferricyanide.

Table 1. The control program of AuNPs-luminol-potassium ferricyanide SIA-CL detection of AA-I.

Device	Command	Parameter	Action
Loop Start (♯) 1	Counter clockwise	45%	Pump filled with carrier
Next sample	Delay (s)	25
Peristaltic pump	Peristaltic pump off
Detector	ON
Syringe pump	Valve position IN
Syringe pump	Set flow rate (μL s^−1)	100
Syringe pump	Aspirate (μL)	1500
Syringe pump	Delay until done
Multiposition valve	Set valve position	3
Syringe pump	Set flow rate (μL s^−1)	100
Syringe pump	Aspirate (μL)	50	(Luminol 2.0 × 10^−4  mol L^−1)
Multiposition valve	Set valve position	2
Syringe pump	Set flow rate (μL s^−1)	100
Syringe pump	Aspirate (μL)	30	(Gold nanoparticles)
Multiposition valve	Set valve position	5
Syringe pump	Set flow rate (μL s^−1)	100
Syringe pump	Aspirate (μL)	50	(Sample (AA-I)
Syringe pump	Delay until done
Multiposition valve	Set valve position	4
Syringe pump	Set flow rate (μL s^−1)	100
Syringe pump	Aspirate (μL)	30	(Potassium ferricyanide 1.0 × 10^−2  mol L^−1)
Syringe pump	Delay until done
Multiposition valve	Detector	7
Syringe pump	Set flow rate (μL s^−1)	100
PMT	Start scan
Syringe pump	Empty
Syringe pump	Delay until done
PMT	Stop scans
Refresh plat
Loop end

Table 2. Performance data obtained from the determination of AA-I using AuNPs-luminol-potassium ferricyanide system.

Analytical characteristics	Obtained results
Linear range, ng mL^−1	10–20,000
Detection limit, ng mL^−1	3
Quantification limit, ng mL^−1	10
Intercept on the ordinate	5722.16
Slope	30.45
%RSD for 25 ng mL^−1 (n = 12)	1.2 %
Correlation coefficient, r	0.9992

Figure 8. Comparative CL signals using luminol-ferricyanide, luminol-ferricyanide-AA-I, luminol-ferricyanide-AuNPs and luminol-ferricyanide-AuNPs-AA-I: Optimum conditions: 50 µL of 2.0 × 10⁻⁴ mol L⁻¹ luminol; 30 µL of AuNPs and 30 µL of 1.0 × 10⁻² mol L⁻¹ potassium ferricyanide and 50 µL sample AA-I.

Scheme 1. The mechanism of CL reaction of luminol-ferricyanide in the presence of AuNPs.

Table 3. Tolerable concentration level of interference to 25 ng mL⁻¹ AA-I.

Interferents	Tolerable level μg mL^−1
Na^+, K^+, Mg^2+, Cl^−, , and	1000
Glucose, sucrose, lactose, talc, starch	500
Aristolochic acid II, uric acid, magnesium stearate, citric acid	125
Adrenaline, dopamine, cystine, histamine, tyrosine	220
Menthol, menthone, pulegone, piperitone and carvacrol acetate	300

Table 4. Intra-day and inter-day precision using enhanced AuNPs-SIA-CL method for detection of AA-I.

Concentration (ng mL^−1 )	Precision % RSD
	Intra-day	Inter-day
50	1.3	1.8
100	1.2	1.4
500	1.5	1.6
800	1.1	1.3
1000	2.0	1.7
1500	1.8	1.5
5000	0.9	1.2
6000	1.1	1.1
8000	0.8	0.9

Table 5. Determination of AA-I am using AuNPs-luminol-potassium ferricyanide SIA-injection CL detection in pure solution and medicinal products.

Sample	Proposed method			Reported method ( 9)
	Taken (ng mL^−1)	Found (ng mL^−1)	% Recovery	Taken (ng mL^−1)	Found (ng mL^−1)	% Recovery
Pure solution	10	9.9	99.0	0.4	0.39	97.5
	100	99.8	99.8	1.0	0.99	99.0
	500	498.5	99.7	10	9.90	99.0
	1000	999.6	99.9	100	99.10	99.1
	5000	4917.3	98.3	400	389.14	97.3
	10,000	9939.2	99.4	600	597.12	99.5
	20,000	19,967.8	99.8
Mean ± SD	99.4 ± 0.6			98.6 ± 0.9
Variance	7			6
%SE	0.36			0.81
%RSD	0.23			0.37
t-test	0.60			0.91
F-test	1.836 (2.201)^a
	2.25 (4.39)^a
Slimming products	10	9.8	98.0	0.4	0.4	100.0
	100	99.8	99.8	1.0	0.98	98.0
	500	498.2	99.6	10	9.90	99.0
	1000	987.6	98.8	100	99.15	99.1
	8000	798.5	99.8	400	389.18	97.3
	10,000	9915.8	99.2	600	597.10	99.5
	20,000	19724.2	98.6
Mean ± SD	99.1 ± 0.7			98.8 ± 0.9
n	7			6
Variance	0.49			0.81
%SE	0.26			0.37
%RSD	0.71			0.91
t-test	0.663 (2.201)^a
F-test	1.65 (4.39)^a

^aFigures in parentheses are the tabulated values of t- and F-testes at 95% confidence limit ( 32).

Table 6. Detection results of AA-I in five medicinal plants using AuNPs enhanced SIA-CL method (n = 6) and confirmed by reported HPLC method ( 9).

Aristolochia Species	Proposed CL-method		Reported HPLC method ( 9)
	AA-I		AA-I
	Mean content (μg/g)	%RSD	Mean content (μg/g)	%RSD
Aristolochia fangchi	19.8	0.8	17.5	0.2
Aristolochia contorta	18.9	1.4	18.0	0.9
Aristolochia debilis	12.5	1.1	10.8	1.2
Aristolochia mandshuriensis	14.6	0.9	11.5	1.1
Asarum	19.3	1.5	18.8	0.8

Yiming, L.; Aihua, L.; Zhifeng, W.; Runmei, O.; Haiding, H. Biomed. Chromatogr. 2010, 24, 174–179. doi: 10.1002/bmc.1267

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