Stability-Indicating HPLC Determination of Gemcitabine in Pharmaceutical Formulations

Table 8

Comparison between analytical methods.

S. number	Analytical method (reference)	Drugs	Column	Detection ()	Silent features and advantages.	Disadvantage
1	HPLC-PDA (Jansen et al., 2000) [3]	Gemcitabine	Zorbax C-8 (5 μm, 4.6 × 250 mm)	275 nm	Sensitive, simple method applicable for separation of drug and degraded products. Degradated products were identified using spectroscopy.	Gradient elution. Only the degradated products of acidic stress studies were separated. Run time: 20 min.
2	HPLC (Rao et al., 2007) [6]	Gemcitabine	ODS column (5 µm, 4.6 × 250 mm)	234 nm	Linearity range: 1–300 µg/mL.	High organic waste (70% acetonitrile). Stability studies not performed.
3	HPLC (Xu et al., 2014) [7]	Gemcitabine and curcumin	Phenomenex C-18 (5 μm, 4.6 × 250 mm)	270 nm (Gem.); 420 nm (curcumin)	LOD: 0.012 µg/mL LOQ: 0.038 µg/mL.; Linearity range: 0.038–1.5 µg/mL.; Sensitive, accurate, and precise method, developed using design of experiment.	Gradient elution, narrow range of linearity, run time: 15 min. Nonstability indicating method (effect of pH and oxidation, exposure to sunlight or UV light, was not studied).
4	HPLC (Mastanamma et al., 2010) [11]	Gemcitabine	C-18 (5 μm, 4.6 × 250 mm)	270 nm	Linearity range: 10–60 µg/mL. Simple and rapid stability indicating method.	Organic waste (40%, methanol) and low sensitivity.
5	HPLC (Kudikala et al., 2014) [12]	Gemcitabine	Enable C18G column (5 µm, 4.6 × 250 mm)	285 nm	LOQ: 1 µg/mL. Linearity range: 1–45 µg/mL. Simple stability indicating method.	Hydrolytic (aq.) and oxidative degraded products not studied. Gemcitabine shows high tailing factor.
6	HPLC (Devanaboyina et al., 2014) [13]	Gemcitabine	Kromasil (5 µm, 4.6 × 150 mm)	247 nm	Linearity range: 50–300 µg/mL.	High organic waste (30% acetonitrile). Stability studies not performed.
7	HPLC (Rajesh et al., 2011) [10]	Gemcitabine Capecitabine	Intersil 3, C-18 column (5 µm, 4.6 × 150 mm)	260 nm	Linearity range: 10–50 µg/mL.	High organic waste (70% acetonitrile). Stability studies not studied.
8	HPLC (Lanz et al., 2007) [14]	Gemcitabine	C18 (3 µm particle size, 4.6 mm × 100 mm)	276 nm	LOQ: 0.02 µg/mL.; Linearity range: 0.02–20 µg/mL.; Sensitive method for analysis of drug in plasma and serum.	Gradient elution, run time: 17 min. Applicable only for serum and plasma samples. Effect of pH, oxidation, or light on stability of raw material/formulation is not studied.
9	LC-MS-MS (Nussbaumer et al., 2010) [28]	Gemcitabine and other anticancer drugs	—	Mass spectrometry (MS-MS)	LOQ: 0.25.; Linearity range: 0.25–2 ng/mL.; Sensitive, simple method applicable for detection of several drugs.	Lower accuracy (85–110%) and precision (15%). Applicable for bioequivalence and pharmacokinetic studies where 15% precision is permitted. Gradient elution, run time: 21 min.
10	HPTLC (Borisagar et al., 2012) [5]	Gemcitabine	—	268 nm	Linearity range: 500–3000 ng/spot.; Rapid HPTLC method for analysis. Stability indicating method.	—
11	Proposed HPLC method	Gemcitabine	Phenomenex Luna C-18 column (5 µm, 4.6 × 250 mm)	275 nm	LOD: 0.15 µg/mL. Linearity ranges from 0.5 to 50 µg/mL.; Isocratic, economical (less organic waste), efficient stability indicating method. Capable of separating different hydrolytic and oxidative products of drug which can be estimated separately. Symmetrical peak shape.	Degraded products are separated but not quantized.