SPDS Set 1 ERP Book

CHON-002

• Extraction was assumed to be finished upon complete disintegration of the tablet in water. Data was not presented for determination of complete disintegration. • Samples were filtered using unspecified filter paper. Filter recovery studies were not reported. • pH is critical for the success of this type of analysis. Data was not given for leading or terminating solutions at various pH levels. • Authors used enzymes for the digestion of CS. The chondroitinase is pH, concentration and temperature dependent. The authors did not describe the sample preparation in the original paper. They did however, discuss following the procedure published by Volpi in 2007 with some modifications. It’s not clear if these modifications were consistent. Miscellaneous typos, cation vs anion among others. The method lacks details for step by step sample preparation used for analysis. This could be due to the 10-page limitation for articles to be included in this particular journal. Sample preparation dilution on p. 59 appears to be out of the calibration curve but in Table 3 the validation samples were stated to be diluted into the calibration curve range. It’s unclear if this was done with routine samples as well. Sample filtration was performed with an unspecified filter type. Filter studies not mentioned. Method was used to test multiple dosage forms but the validation was only for tablets. There is no suggested system suitability requirements. The method refers to analysis of CS but sample concentration estimation appears to be based on CS-A during the validation. It’s unclear which reference material are used in the preparation of stock and working standards, page 59 P2.

Method Clarity

No dangerous chemicals required Simple sample preparation in water Short analysis time

Pros/Strengths

In general, CE has some drawbacks: • Low sensitivity • Sample concentrations must be dramatically increased to obtain the same S/N compared to a typical LC run • pH in the capillary can be affected resulting in countering of the stacking effect. • Lack of data regarding standard retention times and peak area

Cons/Weaknesses

o Inability to quantify analyte o Irreproducible flow rates o Inconsistent injection volumes