Objective: To establish a content determination method for 14 components in pine needles of different varieties and origins simultaneously by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-QQQ MS/MS). Methods: The UPLC-QQQ MS/MS was adopted. A Waters ACQUITY UPLC BEH HILIC (100 mm×2.1 mm,1.7 μm) chromatographic column was used, with a column temperature of 35 ℃. The mobile phase was a mixture of 0.1% formic acid-acetonitrile solution (A) and 0.1% formic acid-aqueous solution (B) for gradient elution, with a flow rate of 0.2 mL·min-1. Electrospray ionization was used, and multiple reaction monitoring mode was employed. The monitored ion pairs of each component were m/z 125.0/79.1(gallic acid), m/z 105.1/77.2(p-hydroxybenzyl alcohol), m/z 109.1/91.1(protocatechuic acid), m/z 93.1/65.2(p-hydroxybenzoic acid), m/z 190.9/85.2(chlorogenic acid), m/z 151.8/108.2(vanillic acid), m/z 135.1/89.2(caffeic acid), m/z 167.0/122.9(syringic acid), m/z 119.2/93.2(p-coumaric acid), m/z 208.1/193.0(sinapic acid), m/z 82.0/77.2(benzoic acid), m/z 91.3/65.3(phenylacetic acid), m/z 93.1/65.2(salicylic acid), and m/z 103.2/77.2(cinnamic acid). Results: The content ranges of each component in the 12 determined pine needle samples were as follows: gallic acid 0.34-3.42 mg·g-1, p-hydroxybenzyl alcohol 1.32-9.76 mg·g-1, protocatechuic acid 0-6.32 mg·g-1, p-hydroxybenzoic acid 0-19.06 mg·g-1, chlorogenic acid 0-18.78 mg·g-1, vanillic acid 0.16-3.81 mg·g-1, caffeic acid 0-6.68 mg·g-1, syringic acid 0.09-4.64 mg·g-1, p-coumaric acid 0.10-9.90 mg·g-1, sinapic acid 0.98-19.01 mg·g-1, benzoic acid 1.28-18.21 mg·g-1, phenylacetic acid 0.95-20.72 mg·g-1, salicylic acid 0-3.25 mg·g-1, and cinnamic acid 0-0.27 mg·g-1. Each component had a good linear relationship within the test range, and the average sample recovery rate was between 98.0% and 101.7%. The quantitative limits of the 14 components were between 0.01 and 0.4 ng. Conclusion: This method is applicable for the determination of phenolic acids in common pine needles, in which 9 compounds, including p-hydroxybenzyl alcohol, chlorogenic acid, vanillic acid, syringic acid, p-coumaric acid, sinapic acid, benzoic acid, salicylic acid, are determined for the first time in pine needles, which can provide reference for the determination of various phenolic acids in pine needles.
WANG Xin
,
LI Bin
,
XIN An-qi
,
WANG Meng-fan
,
MA Qu-huan
,
LIU Xing-guo
,
SHI Xiao-feng2**
. Simultaneous determination of 14 components in pine needles by using UPLC-QQQ MS/MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2024
, 44(10)
: 1713
-1721
.
DOI: 10.16155/j.0254-1793.2024-0247
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