Microwave-accelerated derivatization for the simultaneous gas chromatographic–mass spectrometric analysis of natural and synthetic estrogenic steroids

Zuo, Yuegang; Zhang, Kai; Lin, Yuejuan

doi:10.1016/j.chroma.2007.03.037

Cited by 100 publications

(57 citation statements)

References 37 publications

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“…The peak identification and purity verification was performed by employing a Hewlett -Packard (HP) model GC 5890 Series II gas chromatograph coupled with an HP 5971 series mass selective detector and an HP 7673 GC autosampler [15,16]. Samples were separated on a DB-5 fused-silica capillary column (30 m60.32 mm id, 0.25 lm film, J & W Scientific, Folsom, CA, USA).…”

Section: Cocaine Analysismentioning

confidence: 99%

An accurate and nondestructive GC method for determination of cocaine on US paper currency

Zuo¹,

Zhang

et al. 2008

J of Separation Science

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The presence of cocaine on US paper currency has been known for a long time. Banknotes become contaminated during the exchange, storage, and abuse of cocaine. The analysis of cocaine on various denominations of US banknotes in the general circulation can provide law enforcement circles and forensic epidemiologists objective and timely information on epidemiology of illicit drug use and on how to differentiate money contaminated in the general circulation from banknotes used in drug transaction. A simple, nondestructive, and accurate capillary gas chromatographic method has been developed for the determination of cocaine on various denominations of US banknotes in this study. The method comprises a fast ultrasonic extraction using water as a solvent followed by a SPE cleanup process with a C(18) cartridge and capillary GC separation, identification, and quantification. This nondestructive analytical method has been successfully applied to determine the cocaine contamination in US paper currency of all denominations. Standard calibration curve was linear over the concentration range from the LOQ (2.00 ng/mL) to 100 microg/mL and the RSD less than 2.0%. Cocaine was detected in 67% of the circulated banknotes collected in Southeastern Massachusetts in amounts ranging from approximately 2 ng to 49.4 microg per note. On average, $5, 10, 20, and 50 denominations contain higher amounts of cocaine than $1 and 100 denominations of US banknotes.

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Section: Cocaine Analysismentioning

confidence: 99%

An accurate and nondestructive GC method for determination of cocaine on US paper currency

Zuo¹,

Zhang

et al. 2008

J of Separation Science

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“…[16][17][18][19][20][21] Reversed-phase HPLC methods with a highly aqueous mobile phase have been increasingly attractive in light of the recent movement of green analytical chemistry, which encourages the development of analytical methods without or with reduced consumption of organic solvent, energy and time. [17][18][19][22][23][24] However, many studies have reported that the use of a highly aqueous mobile phase (>90% water) with C18 and C8 columns causes an anomalous chromatographic behavior, and a retention loss of analytes. 19,25 These anomalies have been attributed to (i) aggregation of the bonded hydrocarbon chains in the presence of a highly aqueous mobile phase, rendering them inaccessible to analytes, and (ii) extrusion of the highly aqueous mobile phase from the pores of the particles of the stationary phase.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous Determination of Creatinine and Uric Acid in Human Urine by High-Performance Liquid Chromatography

et al. 2008

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An environmentally friendly reversed-phase HPLC method for simultaneous determination of creatinine and uric acid in human urine samples has been developed. Human urine samples were pretreated by dilution, protein precipitation, centrifugation and filtration, followed by HPLC separations using a reversed-phase C18 column with an aqueous mobile phase of phosphate buffer. The retention loss of a C18 column when using the highly aqueous mobile phases was avoided by employing a gradient elution using a small volume (<0.23 mL) of acetonitrile and phosphate buffer at pH 4.75. This developed method provides a simple, rapid separation and sensitive detection for the species of interest in 10 min with UV detection at 205 nm. Quantitation was carried out by relating the peak areas of the identified compounds to that of hypoxanthine as an internal standard. The detection limits for creatinine and uric acid were 0.045 and 0.062 mg mL -1 , respectively. The recoveries of the standards added to urine samples were 87.3 -102.2% for creatinine and 97.3 -108.6% for uric acid, and the relative standard deviation for both analytes was less than 1.0%. This method has been successfully applied to estimating of creatinine and uric acid in human urine.

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“…In this study, three kinds of sex hormones were simultaneously determined instead of only one kind of specific sex hormone in some literature [27,30,32,33]. Some parameters affecting the MAD, such as derivatization time, microwave power, and reaction solvent, were investigated.…”

Section: Optimization Of Mad Conditionsmentioning

confidence: 99%

Microwave‐accelerated derivatization prior to GC‐MS determination of sex hormones

Zhao

Zhang

et al. 2011

J of Separation Science

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A new microwave-accelerated derivatization method was developed for rapid determination of 13 natural sex hormones in feeds. Sex hormones were isolated from the sample matrix by ultrasonic extraction, followed by solid-phase extraction, derivatized under microwave irradiation, and then analyzed directly by gas chromatography-mass spectrometry (GC-MS) in selective ion monitoring (SIM) mode. The key parameters affecting derivatization efficiency, including microwave irradiation time, microwave power, and reaction solvent were studied. Under microwave power of 360 W and microwave irradiation for 3 min, 13 natural sex hormones were simultaneously derivatized using heptafluorobutyric acid anhydride (HFBA) as derivatization reagent. This method was applied to the determination of 13 natural sex hormones in different feed samples, and the obtained results were compared with those obtained by the traditional thermal derivatization. The recoveries from 58.1 to 111% were obtained at sex hormone concentrations of 10-300 μg/kg with RSDs ≤12.0%. The results showed that the proposed method was fast, simple, efficient and can be applied to the determination of 13 natural sex hormones in different feed samples.

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Microwave-accelerated derivatization for the simultaneous gas chromatographic–mass spectrometric analysis of natural and synthetic estrogenic steroids

Cited by 100 publications

References 37 publications

An accurate and nondestructive GC method for determination of cocaine on US paper currency

An accurate and nondestructive GC method for determination of cocaine on US paper currency

Simultaneous Determination of Creatinine and Uric Acid in Human Urine by High-Performance Liquid Chromatography

Microwave‐accelerated derivatization prior to GC‐MS determination of sex hormones

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