Validation of high-performance liquid chromatography (HPLC) method for quantitative analysis of histamine in fish and fishery products

Nitrofurans residue in fishery products were dangerous for human health and still remain a big challenge in China. However, there are a few available methods to detect nitrofurans residue in fishery products. This study aimed at developing a high performance liquid chromatography (HPLC) method to detect four nitrofurans (furaltadone, nitrofurazone, nitrofurantoin and furazolidone) residue in fishery products sensitively . Firstly the nitrofurans were extracted from samples with ethyl acetate and then concentrated with rotary evaporator. After mobile phase dissolved and normal hexane defatted, the analytes were quantified with an external standard method by HPLC. The results showed that the linear range was 0.025~1.000μg/mL with correlation coefficients all more than 0.998 and the quantification limits of furaltadone, nitrofurazone, nitrofurantoin, furazolidone, were 11.0, 6.00, 13.0 and 7.00μg/kg respectively. The method was used to detect the nitrofurans in fishery products prepared with recovery rates from 72.2% to 107.4% and relative standard deviation (RSD) varied from 6.2% to 10.4%. Therefore, this method can be used for monitoring nitrofurans in commercial fishery products, improving the safety of commercial fishery products in China.

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Formulation and Quantitative Analysis of Betamethasone Valerate and Neomycin Sulfate Cream by High Performance Liquid Chromatography and Spectrophotometry

Open Access Macedonian Journal of Medical Sciences ◽

10.3889/oamjms.2019.516 ◽

2019 ◽

Vol 7 (22) ◽

pp. 3841-3846

Author(s):

Yade Metri Permata ◽

Muchlisyam Bachri ◽

Julia Reveny ◽

Fitri Mardiyanti Sibuea

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Quantitative Analysis ◽

Vitamin E ◽

Stearic Acid ◽

Mobile Phase ◽

High Performance ◽

Hplc Method ◽

Betamethasone Valerate ◽

Neomycin Sulfate

BACKGROUND: Combination of betamethasone valerate and neomycin sulfate in cream is used to treat the itching, redness, dryness, scaling, inflammation and discomfort of various skin conditions caused by infection. The combination of active ingredients has side effects which can cause dry skin, thinning of the skin, hypertrichosis, and stretch marks. AIM: The purpose of this study was to make a formula containing vitamin E and quantitative analysis of betamethasone valerate and neomycin sulfate in creams using High Performance Liquid Chromatography and Spectrophotometry Area Under Curve methods. METHODS: Cream preparation includes smelting and emulsification processes, with oil phases namely stearic acid and vitamin E as well as water phases are glycerin, sodium bi-borate, tri-ethanolamine. Physical tests for the cream were organoleptic, homogeneity, pH, evaluation of dispersion, and viscosity. HPLC analysis for cream was carried out using C18 column, and the mobile phase of methanol: water with comparison optimization beforehand. Spectrophotometry analysis for cream was carried out using application of Area Under Curves methods. RESULTS: The formula used was betamethasone valerate 5 mg, neomycin sulfate 25 mg, stearic acid, glycerin, sodium bi-borate, tri-ethanolamine, vitamin E and distilled water. The obtained cream was in the form of semi-solid, odorless, white (colorless), homogeneous, pH 7, the dispersion power of 500 mg cream is 4.0-4.3 cm in diameter and viscosity is 7500 Cps. Analysis of the determination of the levels of the two components was carried out by the HPLC method C-18 column with the mobile phase of methanol: water (90: 10). Betamethasone valerate and neomycin sulfate levels in formulas made HPLC methods were 94.15%, and 136.56%, respectively and using AUC spectrophotometry methods were 107.98% and 94.81%. CONCLUSION: Cream that made by new formula with vitamin E shows good result in physical evaluation. HPLC methods with a mobile phase of methanol: water (90:10) was not recommended, while the AUC spectrophotometry method shows the valid result of quantitative analysis of betamethasone valerate and neomycin sulfate in cream.

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