Method validation of amlodipine and atorvastatin by liquid chromatography–mass spectrometry (LC–MS) method in human plasma

Figures & data

Figure 1. Structural formulae for (A) amlodipine (MW = 408.9) and (B) atorvastatin (MW = 558.7).

Table 1. Within-run variations and accuracy of the LC–Mass method for quantitation of amlodipine (n = 3)

Nominal added concentration (ng/mL)	Sample number	Measured concentration (ng/mL)	Mean (SD)	CV %
0.1	1	0.099	0.098 (0.0035)	3.55
	2	0.095
	3	0.102
5	1	4.89	5.00 (0.11)	2.29
	2	5.12
	3	5.01
10	1	10.11	9.92 (0.16)	1.64
	2	9.81
	3	9.85

Table 2. Within-run variations and accuracy of the LC–Mass method for quantitation of atorvastatin (n = 3)

Nominal added concentration (ng/mL)	Sample number	Measured concentration (ng/mL)	Mean (SD)	CV %
0.2	1	0.19	0.21 (0.02)	9.52
	2	0.23
	3	0.21
10	1	10.25	10.04 (0.18)	1.86
	2	9.89
	3	9.98
20	1	19.51	20.38 (0.76)	3.73
	2	21.02
	3	20.58

Table 3. Between-run variations and accuracy of the LC–Mass method for quantitation of amlodipine (n = 3)

Nominal added concentration (ng/mL)	Run number	Measured concentration (ng/mL)	Mean (SD)	CV %
0.1	1	0.98	0.97 (0.02)	2.67
	2	1.02
	3	0.97
5	1	4.87	5.10 (0.2)	3.96
	2	5.23
	3	5.21
10	1	10.21	10.13 (0.23)	2.31
	2	9.87
	3	10.32

Table 4. Between-run variations and accuracy of the LC–Mass method for quantitation of atorvastatin (n = 3)

Nominal added concentration (ng/mL)	Run number	Measured concentration (ng/mL)	Mean (SD)	CV %
0.2	1	0.18	0.19 (0.02)	10.58
	2	0.19
	3	0.22
10	1	10.31	10.01 (0.26)	2.56
	2	9.87
	3	9.86
20	1	20.38	20.07 (0.26)	1.29
	2	19.98
	3	19.89

Table 5. Relative recovery of amlodipine by the LC–Mass method (n = 3)

Nominal added concentration (ng/mL)	Sample number	Recovery (%)	Mean (SD)	CV %
0.1	1	90.11	95.17 (4.40)	4.62
	2	97.32
	3	98.09
5	1	97.20	94.08 (4.33)	4.59
	2	89.14
	3	95.89
10	1	101.00	96.47 (6.46)	6.69
	2	99.34
	3	89.08

Table 6. Relative recovery of atorvastatin by the LC–Mass method (n = 3)

Nominal added concentration (ng/mL)	Sample number	Recovery (%)	Mean (SD)	CV %
0.2	1	93.19	93.62 (3.18)	3.4
	2	90.67
	3	97.00
10	1	89.09	95.34 (6.93)	7.27
	2	94.14
	3	102.81
20	1	91.00	94.71 (7.53)	7.95
	2	103.39
	3	89.76

Table 7. Data showing stability of amlodipine in human plasma at different QC levels (n = 5)

	0.1 (ng/mL)	5 (ng/mL)	10 (ng/mL)
Short-term stability	91.18	91.2	90.18
Freeze and thaw stability	92.3	94.01	95.21
Long-term stability	96.15	93.65	95.58
Post-preparative stability	97.14	91.87	91.14

Table 8. Data showing stability of atorvastatin in human plasma at different QC levels (n = 5)

	0.2 (ng/mL)	10 (ng/mL)	20 (ng/mL)
Short-term stability	95.57	90.65	95.65
Freeze and thaw stability	96.56	93.25	94.73
Long-term stability	93.61	94.52	95.94
Post-preparative stability	91.65	92.31	91.57