Development and Single-Laboratory Validation of an Improved Method for the Determination of Cyclamate in Foods Using Liquid Chromatography/Tandem Mass Spectrometry

2014 ◽  
Vol 97 (6) ◽  
pp. 1651-1655 ◽  
Author(s):  
Romina Shah ◽  
Lowri S De Jager ◽  
Timothy H Begley
Keyword(s):  
Internal Standard ◽  
Pomegranate Juice ◽  
Spectral Determination ◽  
Precision Data ◽  
Mass Spectral ◽  
Minimal Sample ◽  
Accuracy And Precision ◽  
Liquid Chromatography Tandem Mass ◽  
Potential Matrix

Abstract A fast and reliable LC-MS/MS method for the determination of cyclamate in a variety of food matrices was developed and validated. This method provides both quantitation and qualitative mass spectral determination important for analysis of regulatory samples. Utilization of a cyclamate-d11 internal standard corrects for potential matrix interferences during sample injection and allows minimal sample preparation. Seventeen commercially available food products were fortified at 250 μg/mL and tested as part of the method validation. Recoveries ranged from 72 to 110%, with RSDs ranging from 3 to 15%. The linear range spanned 0.010–1.00 μg/mL. LODs were 0.1 and 0.6 ng/mL, determined in pomegranate juice and dried fig, respectively. LOQs were 0.3 and 1.6 ng/mL, which are significantly lower than needed to measure cyclamate when used as a food additive. The interday and intraday accuracy and precision data are presented. This method was validated for analysis of a variety of commonly adulterated products, including drinks, dried fruits, jams, and hard candies.

scholarly journals Determination of Ephedrine Alkaloids in Human Urine and Plasma by Liquid Chromatography/Tandem Mass Spectrometry: Collaborative Study

2003 ◽  
Vol 86 (4) ◽  
pp. 643-656 ◽  
Author(s):  
William A Trujillo ◽  
Wendy R Sorenson ◽  
D Gray ◽  
J Laurensen ◽  
G Luo ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Human Urine ◽  
Collaborative Study ◽  
Internal Standard ◽  
Tandem Mass ◽  
Accuracy And Precision ◽  
Liquid Chromatography Tandem Mass ◽  
Negative Controls ◽  
Different Levels

Abstract A collaborative study was conducted to evaluate the accuracy and precision of a method for ephedrine-type alkaloids (i.e., norephedrine, norpseudoephedrine, ephedrine, pseudoephedrine, methylephedrine, and methylpseudoephedrine) in human urine and plasma. The amount of ephedrine-type alkaloids present was determined using liquid chromatography (LC) with tandem mass selective detection. The test samples were diluted to reflect a concentration of 5.00–100 ng/mL for each alkaloid. An internal standard was added and the alkaloids were separated using a 5 μm phenyl LC column with an ammonium acetate, glacial acetic acid, acetonitrile, and water mobile phase. Eight blind duplicates of human urine and eight blind duplicates of human plasma were analyzed by 10 collaborators. In addition to negative controls, test portions of urine and plasma were fortified at 3 different levels with each of the 6 ephedrine-type alkaloids at approximately 1, 2, and 5 μg/mL for urine and 100, 200, and 500 ng/mL for plasma. On the basis of the accuracy and precision results for this collaborative study, it is recommended that this method be adopted Official First Action for the determination of 6 different ephedrine-type alkaloids in human urine and plasma.

scholarly journals Simplified and Rapid Determination of Primaquine and 5,6-Orthoquinone Primaquine by UHPLC-MS/MS: Its Application to a Pharmacokinetic Study

Molecules ◽  
2021 ◽  
Vol 26 (14) ◽  
pp. 4357
Author(s):  
Waritda Pookmanee ◽  
Siriwan Thongthip ◽  
Jeeranut Tankanitlert ◽  
Mathirut Mungthin ◽  
Chonlaphat Sukasem ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
High Performance ◽  
Rapid Determination ◽  
Active Metabolites ◽  
Chromatography Tandem Mass Spectrometry ◽  
Accuracy And Precision ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Isocratic Mode

The method for the determination of primaquine (PQ) and 5,6-orthoquinone primaquine (5,6-PQ), the representative marker for PQ active metabolites, via CYP2D6 in human plasma and urine has been validated. All samples were extracted using acetonitrile for protein precipitation and analyzed using the ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) system. Chromatography separation was carried out using a Hypersil GOLDTM aQ C18 column (100 × 2.1 mm, particle size 1.9 μm) with a C18 guard column (4 × 3 mm) flowed with an isocratic mode of methanol, water, and acetonitrile in an optimal ratio at 0.4 mL/min. The retention times of 5,6-PQ and PQ in plasma and urine were 0.8 and 1.6 min, respectively. The method was validated according to the guideline. The linearity of the analytes was in the range of 25–1500 ng/mL. The matrix effect of PQ and 5,6-PQ ranged from 100% to 116% and from 87% to 104% for plasma, and from 87% to 89% and from 86% to 87% for urine, respectively. The recovery of PQ and 5,6-PQ ranged from 78% to 95% and form 80% to 98% for plasma, and from 102% to from 112% to 97% to 109% for urine, respectively. The accuracy and precision of PQ and 5,6-PQ in plasma and urine were within the acceptance criteria. The samples should be kept in the freezer (−80 °C) and analyzed within 7 days due to the metabolite stability. This validated UHPLC-MS/MS method was beneficial for a pharmacokinetic study in subjects receiving PQ.

Mass spectral determination of long-chain quaternary amines in mixtures

1982 ◽  
Vol 136 ◽  
pp. 135-142 ◽  
Author(s):  
Robert J. Cotter ◽  
Gordon Hansen ◽  
Thomas R. Jones
Keyword(s):  
Spectral Determination ◽  
Mass Spectral ◽  
Long Chain

Determination of Oxadixyl in Wines by Liquid Chromatography-Tandem Mass Spectrometry: Single-Laboratory and Interlaboratory Validation Study

2014 ◽  
Vol 97 (6) ◽  
pp. 1701-1706
Author(s):  
Armen Mirzoian ◽  
Jeffrey R Ammann
Keyword(s):  
Validation Study ◽  
High Throughput Screening ◽  
Multiple Reaction Monitoring ◽  
Direct Injection ◽  
Ionization Source ◽  
Minimal Sample ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Interlaboratory Validation

Abstract A direct injection LC/MS/MS method for the determination of the pesticide oxadixyl in wines was developed and validated. A sample divert valve was used to deliver the fraction that contained oxadixyl to the mass spectrometer's electrospray ionization source. Oxadixyl was monitored and quantitated using two transitions in multiple reaction monitoring mode. The method demonstrated recoveries of 99.2 ± 2.0 and 96.7 ± 5.2% for red and white wines, respectively, a linearity range of 2–20 μg/L, LOD at 0.7 μg/L, LOQ of 2.0 μg/L, and precision values of 8.2% (RSDr) and 6.2% (RSDR). Direct injection of the wine onto a C18 ultra-performance LC column allowed automation and high throughput screening. Benefits of this approach include minimal sample preparation, short (3 min) run times, and the use of matrix-matched calibration standards, which minimize the matrix effect due to interferences from wine phenolics, sugars, and various other components. The method's performance characteristics were not statistically different for white and red wines. An additional interlaboratory validation study involved 12 laboratories and demonstrated good data agreement with HorRat values ranging from 0.23 to 0.52.

scholarly journals Rapid and Sensitive Method for Quantitative Determination of Lopinavir and Ritonavir in Human Plasma by Liquid Chromatography- Tandem Mass Specrtometry

2009 ◽  
Vol 6 (1) ◽  
pp. 223-230 ◽  
Author(s):  
G. A. Temghare ◽  
S. S. Shetye ◽  
S. S. Joshi
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Solid Phase ◽  
Internal Standard ◽  
Therapeutic Monitoring ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Sensitive Method

A rapid and sensitive liquid chromatography-mass spectrometric (LC-MS-MS) method for the simultaneous determination of lopinavir and ritonavir in human plasma using abacavir as internal standard has been developed and validated. Sample preparation of plasma involved solid phase extraction. Detection was performed using an Applied Biosystems Sciex API 2000 Mass spectrometer. The assay of lopinavir and ritonavir was linear over the range of 50 ng mL-1to 20000 ng mL-1and 20 ng mL-1to 3000 ng mL-1 respectively with a precision of <15% and accuracy in the range of 85-115%. The limit of quantification in plasma for lopinavir and ritonavir was 50 ng mL-1and 20 ng mL-1respectively. The described method has the advantage of being rapid and easy and it could be applied in therapeutic monitoring of these drugs in human plasma

Gas Chromatographic Determination of Histapyrrodine Hydrochloride in Pharmaceutical Preparations

1986 ◽  
Vol 69 (4) ◽  
pp. 612-613
Author(s):  
Ramesh T Sane ◽  
Vipul J Doshi ◽  
Sanjay K Joshi ◽  
Vijay K Shastri ◽  
Dhananjay S Sapre ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Chromatographic Determination ◽  
Chlorpheniramine Maleate ◽  
Accuracy And Precision ◽  
Label Claim ◽  
Gas Chromatographic Method

Abstract A simple gas chromatographic method is described for the determination of histapyrrodine HC1 in marketed formulations. Chlorpheniramine maleate is used as the internal standard. The amount of histapyrrodine HC1 found by the proposed method averaged 19.91 mg/tablet, compared with the label claim of 20 mg/tablet. The method was statistically evaluated for accuracy and precision.

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