scholarly journals Determination of Aristolochic Acid in Botanicals and Dietary Supplements by Liquid Chromatography with Ultraviolet Detection and by Liquid Chromatography/Mass Spectrometry: Single Laboratory Validation Confirmation

2006 ◽  
Vol 89 (4) ◽  
pp. 942-959 ◽  
Author(s):  
William A Trujillo ◽  
Wendy R Sorenson ◽  
Paul La Luzerne ◽  
John W Austad ◽  
Darryl Sullivan
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Dietary Supplements ◽  
Aristolochic Acid ◽  
Automation System ◽  
Ultraviolet Detection ◽  
Relative Standard ◽  
Single Laboratory ◽  
Aristolochic Acid I

Abstract The presence of aristolochic acid in some dietary supplements is a concern to regulators and consumers. A method has been developed, by initially using a reference method as a guide, during single laboratory validation (SLV) for the determination of aristolochic acid I, also known as aristolochic acid A, in botanical species and dietary supplements at concentrations of approximately 2 to 32 μg/g. Higher levels were determined by dilution to fit the standard curve. Through the SLV, the method was optimized for quantification by liquid chromatography with ultraviolet detection (LC-UV) and LC/mass spectrometry (MS) confirmation. The test samples were extracted with organic solvent and water, then injected on a reverse phase LC column. Quantification was achieved with linear regression using a laboratory automation system. The SLV study included systematically optimizing the LC-UV method with regard to test sample size, fine grinding of solids, and solvent extraction efficiency. These parameters were varied in increments (and in separate optimization studies), in order to ensure that each parameter was individually studied; the test results include corresponding tables of parameter variations. In addition, the chromatographic conditions were optimized with respect to injection volume and detection wavelength. Precision studies produced overall relative standard deviation values from 2.44 up to 8.26% for aristolochic acid I. Mean recoveries were between 100 and 103% at the 2 μg/g level, between 102 and 103% at the 10 μg/g level, and 104% at the 30 μg/g level.

scholarly journals Multi-Class Determination of 64 Illicit Compounds in Dietary Supplements Using Liquid Chromatography–Tandem Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (19) ◽  
pp. 4399
Author(s):  
Dasom Shin ◽  
Hui-Seung Kang ◽  
Hyungsoo Kim ◽  
Guiim Moon
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Dietary Supplements ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

In this work, liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated for screening and confirmation of 64 illicit compounds in dietary supplements. The target compounds were illegally used pharmaceutical drugs, prohibited compounds, and not authorized ingredients for different therapeutics (sexual enhancement, weight loss, muscular strengthening, and relaxing products). The validation procedure was performed to evaluate selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was >0.98 in the range of 0.5–200 µg L−1. The LOQs were in the range 1–10 µg kg−1 for all target compounds. The accuracy (expressed as recovery) was 78.5–114%. The precision (expressed as the relative standard deviation) was below 9.15%. The developed method was applied for the determination of illicit compounds in dietary supplements collected from websites. As a result, the total detection rate was 13.5% (27 samples detected in 200 samples). The concentrations of detected samples ranged from 0.51 to 226 mg g−1. The proposed methodology is suitable for monitoring the adulteration of illicit compounds in dietary supplements.

scholarly journals Single Laboratory Validation of a Method for Determination of Glucosamine in RawMaterials and Dietary Supplements Containing Glucosamine Sulfate and/or Glucosamine Hydrochloride by High-Performance Liquid Chromatography with FMOC-Su Derivatization

2004 ◽  
Vol 87 (5) ◽  
pp. 1083-1092 ◽  
Author(s):  
Joseph ZiQi Zhou ◽  
Ted Waszkuc ◽  
Felicia Mohammed
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Dietary Supplements ◽  
High Performance ◽  
Raw Materials ◽  
Glucosamine Sulfate ◽  
Glucosamine Hydrochloride ◽  
Relative Standard ◽  
Single Laboratory

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.

scholarly journals Method for the Determination of β-Carotene in Supplements and Raw Materials by Reversed-Phase Liquid Chromatography: Single Laboratory Validation

2004 ◽  
Vol 87 (5) ◽  
pp. 1070-1082 ◽  
Author(s):  
Joseph Schierle ◽  
Bernd Pietsch ◽  
Alan Ceresa ◽  
Christian Fizet ◽  
Edward H Waysek
Keyword(s):  
Liquid Chromatography ◽  
Dietary Supplements ◽  
Raw Materials ◽  
Collaborative Study ◽  
Reversed Phase ◽  
Raw Material ◽  
Relative Standard ◽  
Single Laboratory ◽  
Β Carotene

Abstract A single laboratory validation (SLV) study was conducted for a liquid chromatography (LC) method for the determination of total and all-trans-β-carotene in a variety of dietary supplements, including multivitamin tablets, softgels, capsules, and beadlet raw materials. Extraction variants were developed for the different types of supplements tested based upon the supplement type and level of β-carotene. Water dispersible formulations such as powders, emulsions, tablets, and capsules were enzymatically digested with protease and extracted with dichloromethane–ethanol. Oily suspensions were directly dissolved in dichloromethane–ethanol. After appropriate dilution or concentration, the extracts were chromatographed by using either a reversed-phase C18 column or, in products containing high amounts of α-carotene, a reversed-phase C30 column. The LC systems provided linear responses in the range of 0.1–50 μg β-carotene/mL. The main geometrical isomers of β-carotene (all-trans, 9-cis, 13-cis, and 15-cis) were well separated from each other and from other carotenoids such as α-carotene, cryptoxanthin, lutein, lycopene, and zeaxanthin. Duplicate determinations of total β-carotene performed by 2 technicians in 8 different test materials on 5 different days resulted in relative standard deviations of 1.2–4.4%. Recoveries determined for supplements and beadlet raw material spiked with β-carotene levels of 10 μg to 100 mg/test portion and 0.2–40%, respectively, ranged from 97.5 to 102.1%. On the basis of the accuracy, precision, and recovery results from the SLV study, the method is suggested for a collaborative study on the determination of total and all-trans-β-carotene in dietary supplements.

scholarly journals Determination of the Appetite Suppressant P57 in Hoodia gordonii Plant Extracts and Dietary Supplements by Liquid Chromatography/Electrospray Ionization Mass Spectrometry (LC-MSD-TOF) and LC-UV Methods

2006 ◽  
Vol 89 (3) ◽  
pp. 606-611 ◽  
Author(s):  
Bharathi Avula ◽  
Yan-Hong Wang ◽  
Rahul S Pawar ◽  
Yatin J Shukla ◽  
Brian Schaneberg ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Dietary Supplements ◽  
Reversed Phase ◽  
Ionization Mass ◽  
Active Constituent ◽  
Appetite Suppressant ◽  
Hoodia Gordonii ◽  
Relative Standard

Abstract Hoodia gordonii is traditionally used in South Africa for its appetite suppressant properties. P57AS3 (P57), an oxypregnane steroidal glycoside, is the only reported active constituent from this plant as an appetite suppressant. Effective quality control of these extracts or products requires rapid methods to determine P57 content. New methods of liquid chromatography/mass spectrometry (LC/MS) and LC-UV for analysis of P57 from H. gordonii have been developed. The quantitative determination of P57 was achieved with a Phenomenex Gemini (Torrance, CA) reversed-phase column using gradient mobile phase of water and acetonitrile, both containing 0.1% acetic acid. The method was validated for linearity, repeatability, and limits of detection and quantification. Good results were obtained in terms of repeatability (relative standard deviation <5.0%) and recovery (98.5103.5%). The developed methods were applied to the determination of P57 for H. gordonii plant samples, one related genus (Opuntia ficus-indica), and dietary supplements that claim to contain H. gordonii.

scholarly journals Determination of Chondroitin Sulfate Content in Raw Materials and Dietary Supplements by High-Performance Liquid Chromatography with Ultraviolet Detection After Enzymatic Hydrolysis: Single-Laboratory Validation

2007 ◽  
Vol 90 (3) ◽  
pp. 659-669 ◽  
Author(s):  
David Ji ◽  
Mark Roman ◽  
Joseph Zhou ◽  
Jana Hildreth
Keyword(s):  
Liquid Chromatography ◽  
Chondroitin Sulfate ◽  
Dietary Supplements ◽  
Limit Of Detection ◽  
Raw Materials ◽  
Negative Control ◽  
Sulfate Content ◽  
Ultraviolet Detection ◽  
Relative Standard ◽  
Single Laboratory

Abstract A method to quantify chondroitin sulfate in raw materials and dietary supplements at a range of about 5 to 100% (w/w) chondroitin sulfate has been developed and validated. The chondroitin sulfate is first selectively hydrolyzed by chondroitinase ACII enzyme to form un-, mono-, di-, and trisulfated unsaturated disaccharides; the resulting disaccharides are then quantified by ion-pairing liquid chromatography with ultraviolet detection. The amounts of the individual disaccharides are summed to yield the total amount of chondroitin sulfate in the material. Single-laboratory validation has been performed to determine the repeatability, accuracy, selectivity, limit of detection, limit of quantification, ruggedness, and linearity of the method. Repeatability precision for total chondroitin sulfate content was between 1.60 and 4.72% relative standard deviation, with HorRat values between 0.79 and 2.25. Chondroitin sulfate recovery from raw material negative control was between 101 and 102%, and recovery from finished product negative control was between 105 and 106%.

scholarly journals Determination of Aconitum Alkaloids in Dietary Supplements and Raw Botanical Materials by Liquid Chromatography/UV Detection with Confirmation by Liquid Chromatography/Tandem Mass Spectrometry: Collaborative Study

2009 ◽  
Vol 92 (1) ◽  
pp. 111-118 ◽  
Author(s):  
Siu-Kay Wong ◽  
C T Che ◽  
H-Z Guo ◽  
S Ji ◽  
J-H Kim ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Dietary Supplements ◽  
Collaborative Study ◽  
Uv Detection ◽  
Tandem Mass ◽  
Aconitum Alkaloids ◽  
Relative Standard

Abstract An interlaboratory study was conducted to evaluate a method for the determination of 3 Aconitum alkaloids, viz., aconitine, mesaconitine, and hypaconitine, in raw botanical material and dietary supplements. The alkaloids were extracted with diethyl ether in the presence of ammonia. After cleanup by solid-phase extraction to remove matrix interferences, the alkaloids were determined by reversed-phase liquid chromatography (LC)/UV detection at 235 nm with confirmation by LC/tandem mass spectrometry (MS/MS). A total of 14 blind duplicates were successfully analyzed by 12 collaborators. For repeatability, the relative standard deviation (RSDr) values ranged from 1.9 to 16.7, and for reproducibility, the RSDR values ranged from 6.5 to 33. The HorRat values were all <2 with only one exception at 2.3. All collaborating laboratories had calibration curves with correlation coefficients of >0.998. In addition, 6 collaborators performed the confirmation and were able to verify the identities of the alkaloids by using LC/MS/MS.

scholarly journals Determination of Ubidecarenone (Coenzyme Q10, Ubiquinol-10) in Raw Materials and Dietary Supplements by High-Performance Liquid Chromatography with Ultraviolet Detection: Single-Laboratory Validation

2007 ◽  
Vol 90 (5) ◽  
pp. 1227-1236 ◽  
Author(s):  
Debra Orozco ◽  
Jules Skamarack ◽  
Kelly Reins ◽  
Barry Titlow ◽  
Steve Lunetta ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Dietary Supplements ◽  
Coenzyme Q10 ◽  
High Performance ◽  
Raw Materials ◽  
Biologically Active ◽  
Ultraviolet Detection ◽  
Relative Standard ◽  
Single Laboratory

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.

scholarly journals Liquid Chromatography–Tandem Mass Spectrometry for the Simultaneous Determination of Doxorubicin and its Metabolites Doxorubicinol, Doxorubicinone, Doxorubicinolone, and 7-Deoxydoxorubicinone in Mouse Plasma

Molecules ◽  
2020 ◽  
Vol 25 (5) ◽  
pp. 1254 ◽  
Author(s):  
Won-Gu Choi ◽  
Dong Kyun Kim ◽  
Yongho Shin ◽  
Ria Park ◽  
Yong-Yeon Cho ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Tandem Mass ◽  
Mouse Plasma ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

Doxorubicin, an anthracycline antitumor antibiotic, acts as a cancer treatment by interfering with the function of DNA. Herein, liquid chromatography-tandem mass spectrometry was for the first time developed and validated for the simultaneous determination of doxorubicin and its major metabolites doxorubicinol, doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone in mouse plasma. The liquid–liquid extraction of a 10 μL mouse plasma sample with chloroform:methanol (4:1, v/v) and use of the selected reaction monitoring mode led to less matrix effect and better sensitivity. The lower limits of quantification levels were 0.5 ng/mL for doxorubicin, 0.1 ng/mL for doxorubicinol, and 0.01 ng/mL for doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone. The standard curves were linear over the range of 0.5–200 ng/mL for doxorubicin; 0.1–200 ng/mL for doxorubicinol; and 0.01–50 ng/mL for doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone in mouse plasma. The intra and inter-day relative standard deviation and relative errors for doxorubicin and its four metabolites at four quality control concentrations were 0.9–13.6% and –13.0% to 14.9%, respectively. This method was successfully applied to the pharmacokinetic study of doxorubicin and its metabolites after intravenous administration of doxorubicin at a dose of 1.3 mg/kg to female BALB/c nude mice.

scholarly journals Determination of 7B3 Residues in Cotton Plants by Liquid Chromatography/Mass Spectrometry

2009 ◽  
Vol 92 (1) ◽  
pp. 302-306 ◽  
Author(s):  
Xiao-Jing Yan ◽  
Xiao-Mei Liang ◽  
Yan-Jun Xu ◽  
Shu-Hui Jin ◽  
Dao-Quan Wang
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Cotton Plants

Abstract A method was developed for the determination of 7B3 (12-propyloxyimino-1,15-pentadecanlactam), a novel macrolactam fungicide, by liquid chromatography/mass spectrometry (LC/MS) with positive electrospray ionization (ESI+). The method used a reversed-phase C18 column and acetonitrilewater (60 + 40, v/v) mobile phase. The quick, easy, cheap, effective, rugged, and safe method was used for extraction of 7B3 from cotton plants, which involved the extraction of 10 g homogenized sample with 10 mL acetonitrile, followed by the addition of 4 g anhydrous MgSO4 and 1.0 g NaCl. After centrifugation, 1 mL of the buffered acetonitrile extract was transferred into a tube containing 50 mg primary secondary amine sorbent and 100 mg anhydrous MgSO4. After shaking and centrifugation, the final extract was transferred to an autosampler vial for concurrent analysis by LC/MS. The results of 7B3 determined by LC/MS in the selective ion monitoring mode were linear, and the matrix effect of the method was evaluated. The average recoveries of 7B3 fortified at different levels were within 84.1100.2, and the relative standard deviations were <7.5 for all samples analyzed. The method limit of detection and the limit of quantitation values were 0.03 and 0.1 mg/kg, respectively. The proposed method was successfully applied to determine 7B3 residues in practical samples. This method is sensitive, accurate, reliable, simple, and safe.

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