Determination of ortho-Phenylphenol Residues in Lemon Rind by High-Performance Liquid Chromatography with Electrochemical Detection Using a Microbore Column

Abstract

A simple and highly sensitive method has been developed for determining ortho-phenylphenol (OPP) in lemon rind by high-performance liquid chromatography with electrochemical detection using a microbore column (µHPLC-ECD). Based on the voltammetric behavior of OPP, µHPLC-ECD was established using a CAPCELL PAK C-18 UG 120 microbore ODS column, 17 mM acetic acid-sodium acetate buffer (pH 4.0)/acetonitrile (60/40, v/v) as a mobile phase and an applied potential at +0.9 V vs. Ag/AgCl. The current peak height was found to be linearly related to the amount of OPP injected from 3.4 pg to 1.7 ng (r > 0.999). The detection limit (S/N = 3) was 3.4 pg (20 fmol), which was 100 times greater in terms of sensitivity when compared to conventional HPLC with UV detection. Standard OPP at 0.425 ng was detected with a relative standard deviation (RSD) of 1.9% (n = 10). The OPP contents in several lemon samples were determined by the present method. The recoveries of OPP from lemon rind exceeded 98% with an RSD (n = 5) of less than 3.01%.

Determination of hesperidin in Pericarpium Citri Reticulatae by semi-micro HPLC with electrochemical detection

“…HPLC-ECD is sensitive, inexpensive, and works without complex and timeconsuming sample preparations, as reported by Careri et al [18], Sontag et al [19], and Jin et al [20]. In our previous reports, we successfully developed a more than 30-fold sensitive HPLC-ECD method for determining catechins, quercetin, and ortho-phenylphenol [21][22][23] by using a microbore octadecylsilica (ODS) column. When compared to a reported HPLC-ECD method that used a conventional ODS column [24][25][26], our method would be useful for the quality control of Pericarpium Citri Reticulatae using hesperidin content as a marker.…”

Determination of Honokiol and Magnolol by Micro HPLC with Electrochemical Detection and Its Application to the Distribution Analysis in Branches and Leaves of Magnolia obovata

“…[21][22][23] So, the present HPLC-ECD method using a microbore column (mHPLC-ECD) was expected to be an even more highly sensitive method. In the present study, we developed a mHPLC-ECD method for determining honokiol and magnolol, using diethylstilbestrol ( Fig.…”

“…In our previous reports, we successfully developed a more than 30 fold sensitive HPLC-ECD method for determining catechins 21) and quercetin 22) in human plasma, and orthophenylphenol in lemon rind 23) using a microbore octadecylsilica (ODS) column, when compared to a reported HPLC-ECD method that used a conventional ODS column. [21][22][23] So, the present HPLC-ECD method using a microbore column (mHPLC-ECD) was expected to be an even more highly sensitive method.…”

Simple HPLC–UV Analysis of Phenol and Its Related Compounds in Tap Water after Pre-Column Derivatization with 4-Nitrobenzoyl Chloride

“…2-PP exhibits low acute toxicity in animal experiments [7]. The Japanese government approved its use as a food additive only for citrus fruits in 1977 with the permitted maximum residue level of 10 ppm in whole fruits [8] [9]. The WHO view on the toxicity of 2-PP is as follows [10]: "A health-based value of 1 mg/L can be calculated for 2-PP on the basis of an ADI of 0.4 mg/kg of body weight, based on a NOAEL of 39 mg/kg of body weight per day in a 2-year toxicity study for decreased body weight gain and hyperplasia of the urinary bladder and carcinogenicity of the urinary bladder in male rats, using an uncertainty factor of 100.…”

“…developed a highly sensitive method of 2-PP determination by HPLC with electrochemical detection, using a microbore column; this afforded a detection limit of 3.4 pg [9]. GC-mass spectrometry methods for determination of 2-PP after derivatization with pentafluorobenzoyl bromide and ferrocenecarboxylic acid chloride were applied to beer and citrus fruit samples, respectively [5] [6].…”