Development and Validation of LC-MS/MS for Analyzing Potential Genotoxic Impurities in Pantoprazole Starting Materials

Table 3

Summary of the validation report of the LC-MS/MS method.

Parameter	Impurity C	Impurity D	Impurity E	Impurity F	Impurity G	Impurity H
Linear equation	y = 52.979x + 65.67	y = 11447x − 53046	y = 320.19x + 586.71	y = 541.39x − 3663.8	y = 15.745x + 60.04	y = 1174.6x + 1880.2
R	0.9998	0.9999	0.9988	0.9999	0.9991	1.0000
Linearity range (ng/mL)	20.8∼1042.0	20.3∼1013.0	22.6∼564.5	20.3∼1015.0	50.6∼1012.0	19.8∼988.0
Detection limit (ng/mL)	0.20	0.03	0.10	0.20	1.00	0.05
Quantitation limit (ng/mL)	1.00	0.10	0.50	1.00	5.00	0.20
Precision% (n = 6)	5.82	4.94	3.13	6.17	2.69	5.66
Stability (24 h)	4.91	7.37	1.89	4.47	6.67	4.16
Accuracy at 80% level (n = 3)
% recovery	97.85	94.63	98.36	97.19	97.07	107.43
RSD% (n = 6)	3.67	6.35	3.50	5.83	4.86	1.96
Accuracy at 100% level (n = 3)
% recovery	98.58	98.17	94.32	100.94	95.03	103.63
RSD% (n = 6)	5.06	5.45	3.19	4.85	4.62	0.94
Accuracy at 120% level (n = 3)
% recovery	98.02	97.34	93.42	98.05	102.20	106.29
RSD% (n = 6)	4.05	4.11	3.07	3.35	4.36	1.78