Single-Laboratory Validation of a Method for the Detection and/or Quantification of Select Alkaloids in Goldenseal Supplements and Raw Materials by Reversed-Phase High-Performance Liquid Chromatography

2008 ◽  
Vol 46 (1-2) ◽  
pp. 135-144 ◽  
Author(s):  
Paula N. Brown ◽  
Lori A. Paley ◽  
Mark C. Roman ◽  
Michael Chan
2004 ◽  
Vol 87 (5) ◽  
pp. 1083-1092 ◽  
Author(s):  
Joseph ZiQi Zhou ◽  
Ted Waszkuc ◽  
Felicia Mohammed

Abstract Single laboratory validation of a method for determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by with high-performance liquid chromatography FMOC-Su derivatization. Tests with 2 blank matrixes containing SAMe, vitamin C, citric acid, chondroitin sulfates, methylsulfonylmethane, lemon juice concentrate, and other potential interferents showed the method to be selective and specific. Eight calibration curves prepared over 7 working days indicated excellent reproducibility with the linear range at least over 2.0–150 μg/mL, and determination coefficients >0.9999. Average spike recovery from the blank matrix (n = 8 over 2 days) was 93.5, 99.4, and 100.4% at respective spike levels of 15, 100, and 150%, and from the sample matrix containing glucosamine (n = 3) was 99.9 and 102.8% at respective levels of 10 and 40%, with relative standard deviations <0.9%. The method was also applied to 12 various glucosamine finished products and raw materials. The stability tests confirmed that glucosamine–FMOC-Su derivative once formed is stable at room temperature for at least 5 days. Limit of quantitation was 1 μg/mL and limit of detection was 0.3 μg/mL. The method is ready to proceed for the collaborative study.


2021 ◽  
Vol 284 ◽  
pp. 03002
Author(s):  
Mikhail Sergeev ◽  
Georgiy Zaitsev ◽  
Dmitry Yermolin

In this study, high performance liquid chromatography (HPLC) was used to analyze the protodioscin content in Tribulus terrestris samples. They were separated by C18 chromatography column, gradient with 0.1 % phosphoric acid solution and acetonitrile was used as the mobile phase with the flow rate of 0.5 mL/min, the column temperature was 45 °C, and the detection wavelength was 203 nm. The results showed that the protodioscin content has a good linear correlation (r>0.999) within the range of 50 mg/L to 1500 mg/L. In samples of raw material from Crimea it was found: 0.546 % ± 0.013 protodioscin and in analyzed material from Western Siberia it was 0.338% ± 0.008 for n=3. Raw materials of Tribulus terrestris growing in Crimea are more promising than similar raw materials from the West Siberian region due to the higher content of protodioscin for the production of biologically active products containing steroid saponins.


2007 ◽  
Vol 90 (5) ◽  
pp. 1227-1236 ◽  
Author(s):  
Debra Orozco ◽  
Jules Skamarack ◽  
Kelly Reins ◽  
Barry Titlow ◽  
Steve Lunetta ◽  
...  

Abstract A method based on high-performance liquid chromatography with ultraviolet detection has been developed to quantify ubidecarenone [coenzyme Q10 (CoQ10)] in raw materials and dietary supplements. Single-laboratory validation has been performed on the method to determine repeatability, accuracy, selectivity, limits of detection and quantification (LOQ), ruggedness, and linearity for CoQ10. As CoQ10 can exist as the biologically active reduced form, the application of an oxidizing agent, ferric chloride, drives the equilibrium mechanics to the fully oxidized state and allows for exact quantification of total CoQ10 in the sample. This method was found to be fit and linear for the testing of materials containing CoQ10 in the range of 501000 mg/g. Repeatability precision for CoQ10 was between 2.15 and 5.00 relative standard deviation. Observed recovery of CoQ10 was found to be between 93.8 and 100.9. LOQ was found to be 9 g/mL. Further, limited studies showed that some adulterants and degraded material could be satisfactorily separated from CoQ10 and identified.


Author(s):  
Raju Chandra ◽  
Manisha Pant ◽  
Harchan Singh ◽  
Deepak Kumar ◽  
Ashwani Sanghi

A reliable and reproducible reversed-phase high performance liquid chromatography (RP-HPLC) was developed for the quantitative determination of Remipril drug content from marketed bulk tablets. The active ingredient of Remipril separation achieved with C18 column using the methanol water mobile phase in the ratio of 40:60 (v/v). The active ingredient of the drug content quantify with UV detector at 215 nm. The retention time of Remipril is 5.63 min. A good linearity relation (R2=0.999) was obtained between drug concentration and average peak areas. The limit of detection and limit of quantification of the instrument were calculated 0.03 and 0.09 µg/mL, respectively. The accuracy of the method validation was determined 102.72% by recoveries method.


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