Development of a high-performance liquid chromatography with tandem mass spectrometry method for identifying common adulterant content in saffron (Crocus sativus L.)

Abstract

Objectives This study aimed to develop an efficient and reliable method for estimating common adulterants in saffron by detecting their characteristic components to warrant its efficacy and regular use as a highly valuable medicinal herb. Methods A selective and sensitive high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS) method was developed to estimate the common adulterants in saffron from corn stigma, chrysanthemum and safflower through the simultaneous determination of specific constituents including allantoin, chlorogenic acid (ChA) and hydroxysafflor yellow A (HSYA). Peak identification of each target compound was confirmed from product ions obtained using multiple reaction monitoring triggered enhanced product ions mass chromatogram. Method validation in terms of linearity, sensitivity, reproducibility, accuracy and stability was systematically performed according to official guidelines. Key findings Satisfactory separation of the three components was achieved on a C 18 column (4.6 9 250 mm, 5 lm) with methanol-acetonitrile-ammonium acetate (3.0 mM) as the mobile phase at gradient elution. The identification of these specific constituents was accomplished using the multiple reaction monitoring mode in combination with enhanced product ion supplementary confirmation. The established method was validated in terms of linearity, sensitivity, reproducibility, accuracy and recovery, which were found satisfactory for sensitive detection of the three target compounds. Conclusions By detecting the specific constituents allantoin, ChA and HSYA in one run, the adulterants of corn stigma, chrysanthemum and safflower can be effectively identified and estimated in saffron. This is the first report on developing a simple, sensitive and operational method for the identification and estimation of common adulterants of saffron, that was forwarded for broaden application.

Relationships between amylopectin internal molecular structure and physicochemical properties of starch

“…In 2019, high performance liquid chromatography (HPLC) with tandem mass spectroscopy was used to detect corn stigma, chrysanthemum, and safflower as adulterants in saffron, through the identification of the components of allantoin, chlorogenic acid (ChA) and hydroxysafflor yellow A (HSYA) (Kong et al, 2019). Using this technique, along with gel permeation chromatography (GPC), Sudan dyes were detected in Egyptian spices with a limit of quantification of 0.1 mg/kg (Sebaei et al, 2019).…”

Determination of adulteration, geographical origins, and species of food by mass spectrometry

“…Many scholars have used the LC‐MS approach to discover markers of adulteration of saffron. The allantoin, chlorogenic acid, and hydroxysafflor yellow A content is helpful for the detection of saffron samples adulterated with corn stigma, chrysanthemum, and safflower (Kong et al, 2019). Kaempferol derivatives are authenticity markers and geniposide is an adulteration marker for saffron (Guijarro‐Díez et al, 2017).…”

Detection of botanical adulterants in saffron powder

“…Specifically, it may be undeclared additions of colored stamens [ 4 , 7 – 10 ], styles [ 10 – 12 ], or petals [ 9 , 10 ] of the saffron itself. For this purpose, petals of safflower ( Carthamus tinctorius L.) [ 1 , 2 , 4 , 6 – 8 , 10 – 23 ], petals of calendula ( Calendula officinalis L.) [ 1 , 2 , 4 , 7 , 10 – 13 , 15 , 17 , 20 ], rhizomes of turmeric ( Curcuma longa L.) [ 1 , 2 , 4 , 7 , 8 , 10 , 12 , 15 , 17 , 18 , 20 , 21 , 23 ], extracts of gardenia fruits ( Gardenia jasminoides J. Ellis) [ 1 , 4 , 5 , 7 , 8 , 17 , 24 – 27 ], petals of mountain arnica ( Arnica montana L.) [ 1 , 2 , 15 , 17 ], dye from seeds of achiote ( Bixa orellana L.) [ 2 , 15 , 17 ], petals of chrysanthemum (C hrysanthemum morifolium L.) [ 6 , 16 , 17 ], petals of hemerocallis ( Hemerocallis sp.) [ 2 , 15 , 17 ], stigmas of crocus vernus ( Crocus vernus (L.) Hill) [ 2 , 15 ], dye from pomegranate fruits or petals ( Punica granatum L.) [ 10 , 17 ], dye from flowers of buddleia ( Buddleja officinalis ...…”