Simultaneous Determination of 12 Preservatives in Pastries Using Gas Chromatography–Mass Spectrometry
Abstract
:1. Introduction
2. Materials and Methods
2.1. Instruments and Reagents
2.2. Chromatography–Mass Spectrometry Conditions
2.2.1. Chromatography Conditions
2.2.2. Mass Spectrometry Conditions
2.3. Preparation of Solutions
2.4. Preparation of Standard Curve
2.5. Sample Preparation
2.6. Test of Recovery by Adding Standard
3. Results and Discussion
3.1. Optimization of Detection Conditions
3.1.1. Selection of Internal Standard
3.1.2. Selection of Characteristic Ions
3.1.3. Selection of Chromatographic Column
3.2. Optimization of Sample Preparation Conditions
3.2.1. Selection of Extraction Solvents
3.2.2. Purification Conditions
3.3. Methodological Validation
3.3.1. Linearity, Detection Limit, and Quantification Limit
3.3.2. Accuracy and Precision
3.4. Actual Sample Analysis
4. Conclusions
Author Contributions
Funding
Data Availability Statement
Conflicts of Interest
References
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Compound Name | Standard Series Concentration (μg/mL) | ||||
---|---|---|---|---|---|
Acetic acid, propionic acid, sorbic acid, benzoic acid, dehydroacetic acid | 50 | 25 | 12.5 | 5 | 2.5 |
Dimethyl fumarate, methyl p-hydroxybenzoate, isobutyl ester, butyl ester, Ethyl p-hydroxybenzoate, propyl ester, Isopropyl p-hydroxybenzoate | 20 | 10 | 4 | 2 | 1 |
Food Preservatives | Quantitative Ion (m/z) | Qualitative Ion (m/z) | Retention Time (min) | |
---|---|---|---|---|
Acetic acid | 60 | 43 | 45 | 6.161 |
Propionic acid | 74 | 73 | 57 | 6.875 |
Dimethyl fumarate | 113 | 85 | 59 | 7.011 |
Sorbic acid | 112 | 97 | 67 | 11.342 |
Dehydroacetic acid | 168 | 153 | 85 | 11.626 |
Benzoic acid | 105 | 122 | 77 | 13.280 |
Isopropyl p-hydroxybenzoate | 121 | 138 | 180 | 17.888 |
Methyl p-hydroxybenzoate | 121 | 152 | 93 | 17.967 |
D4-p-hydroxybenzoate | 125 | 142 | 170 | 18.295 |
Ethyl p-hydroxybenzoate | 121 | 138 | 166 | 18.296 |
Propyl p-hydroxybenzoate | 121 | 138 | 180 | 19.618 |
Isobutyl p-hydroxybenzoate | 121 | 138 | 65 | 20.113 |
Butyl p-hydroxybenzoate | 121 | 138 | 194 | 21.469 |
Food Preservatives | Linear Range (μg/mL) | Regression Equation | r² | Detection Limit/(mg/kg) | Quantitative Limit/(mg/kg) |
---|---|---|---|---|---|
Acetic acid | 2.5–50 | y = 5157x − 1600 | 0.9967 | 0.17 | 0.58 |
Propionic acid | 2.5–50 | y = 7128x − 0900 | 0.9993 | 0.60 | 1.99 |
Dimethyl fumarate | 1.0–20 | y = 19,160x + 10,680 | 0.9942 | 0.28 | 0.92 |
Sorbic acid | 2.5–50 | y = 3089x − 263 | 0.9923 | 1.83 | 6.10 |
Dehydroacetic acid | 2.5–50 | y = 4613x − 451 | 0.9904 | 2.00 | 6.67 |
Benzoic acid | 2.5–50 | y = 8941x − 9780 | 0.9924 | 1.38 | 4.62 |
Isopropyl p-hydroxybenzoate | 1.0–20 | y = 31,090x − 634 | 0.9993 | 0.04 | 0.14 |
Methyl p-hydroxybenzoate | 1.0–20 | y = 31,470x + 961.2 | 0.9973 | 0.04 | 0.12 |
Ethyl p-hydroxybenzoate | 1.0–20 | y = 32,140x − 53 | 0.9979 | 0.04 | 0.12 |
Propyl p-hydroxybenzoate | 1.0–20 | y = 30,030x + 669 | 0.996 | 0.11 | 0.36 |
Isobutyl p-hydroxybenzoate | 1.0–20 | y = 32,310x + 18780 | 0.99 | 0.33 | 1.03 |
Butyl p-hydroxybenzoate | 1.0–20 | y = 27,050x − 024 | 0.9974 | 0.05 | 0.18 |
Food Preservatives | Low Concentration (10 mg/kg) | Medium Concentration (40 mg/kg) | High Concentration (100 mg/kg) | |||
---|---|---|---|---|---|---|
Average Recovery Rate | Relative Standard Deviation | Average Recovery Rate | Relative Standard Deviation | Average Recovery Rate | Relative Standard Deviation | |
Acetic acid | 75.85 | 2.37 | 71.19 | 4.08 | 70.18 | 4.05 |
Propionic acid | 79.6 | 4.72 | 77.93 | 2.78 | 70.29 | 3.89 |
Sorbic acid | 90.28 | 2.27 | 81.48 | 3.12 | 80.73 | 1.82 |
Dehydroacetic acid | 78.6 | 3.48 | 76.07 | 4.29 | 73.72 | 6.28 |
Denzoic acid | 86.01 | 3.39 | 83.39 | 2.75 | 81.73 | 5.42 |
Food Preservatives | Low Concentration (4 mg/kg) | Medium Concentration (20 mg/k) | High Concentration (40 mg/kg) | |||
---|---|---|---|---|---|---|
Average Recovery Rate | Relative Standard Deviation | Average Recovery Rate | Relative Standard Deviation | Average Recovery Rate | Relative Standard Deviation | |
Dimethyl fumarate | 107.97 | 5.28 | 98.45 | 2.69 | 85.24 | 9.27 |
Isopropyl p-hydroxybenzoate | 98.32 | 8.44 | 104 | 7.26 | 109.22 | 2.97 |
Methyl p-hydroxybenzoate | 103.79 | 8.98 | 102.91 | 6.72 | 100.21 | 9.79 |
Ethyl p-hydroxybenzoate | 98.97 | 5.48 | 101.73 | 3.43 | 96.48 | 7.73 |
Propyl p-hydroxybenzoate | 102.83 | 8.14 | 101.07 | 8.25 | 98.05 | 8.64 |
Isobutyl p-hydroxybenzoate | 81.82 | 2.85 | 83.87 | 4.3 | 83.28 | 3.91 |
Butyl p-hydroxybenzoate | 106.72 | 6.27 | 107.05 | 5.81 | 87.4 | 9.11 |
Acetic Acid | Propionic Acid | Dimethyl Fumarate | Sorbic Acid | Dehydroacetic Acid | Benzoic Acid | |
---|---|---|---|---|---|---|
Scallion-flavored Soda Cake | 22.23 | 1.02 | ND | ND | 7.39 | 25.69 |
Rice noodles | 10.92 | ND | ND | ND | ND | ND |
Osmanthus Lotus Root Cake | 14.19 | ND | ND | 30.34 | ND | ND |
Corn flour | ND | ND | ND | ND | ND | 4.39 |
Pacific Soda Cake | ND | ND | ND | 6.23 | ND | 4.39 |
Evergreen Crispy Biscuit | ND | ND | 1.85 | ND | ND | ND |
Sugar-free, high-fiber crispy biscuits | ND | ND | ND | ND | ND | ND |
Gangrong Steamed Cake | 6.88 | ND | ND | 520.63 | 114.84 | 14.52 |
Gangrong Steamed Bread | 73.82 | 82.48 | ND | 68.03 | 175.15 | 4.51 |
Gangrong Sandwich Sandwich Cake | 3.64 | ND | ND | 439.19 | 92.48 | ND |
Barbie Bear Pure Cake | 11.20 | 1.88 | ND | 267.05 | 103.93 | ND |
Barbie Bear Fresh Cake | 18.95 | 1.87 | ND | 269.20 | 120.36 | ND |
Hometown Sweet Pork Floss and Cheese Small Rolls | 13.13 | ND | ND | 540.56 | 149.02 | ND |
Hometown Fruit Cake | 4.31 | ND | ND | 537.69 | 171.81 | ND |
Hamburg cake | 17.26 | ND | ND | 347.71 | 127.62 | ND |
White Peach Milk Cake | 14.41 | ND | ND | 381.25 | 90.32 | ND |
Cheese milk cake | 22.35 | ND | ND | 439.79 | 102.59 | ND |
Sucrose-free cake | 9.48 | ND | ND | 360.67 | 111.34 | ND |
Sea salt cheese cake | 40.66 | 2.29 | ND | 346.02 | 105.75 | 3.11 |
Milk vanilla-flavored small cake | 4.14 | ND | ND | 539.48 | 74.59 | ND |
Honey cheese-flavored small cake | 8.91 | ND | ND | 471.85 | 77.00 | ND |
Condensed milk toast | 73.79 | 150.53 | ND | 72.75 | 207.95 | 2.93 |
Purple Rice Toast | 73.35 | 137.54 | ND | 147.31 | 272.68 | ND |
Cheese toast | 72.27 | 142.08 | ND | 80.96 | 217.06 | ND |
Yeast Salty Toast | 66.03 | 122.34 | ND | 137.45 | 225.30 | ND |
Isopropyl P-Hydroxybenzoate | Methyl P-Hydroxybenzoate | Ethyl P-Hydroxybenzoate | Propyl P-Hydroxybenzoate | Isobutyl P-Hydroxybenzoate | Butyl P-Hydroxybenzoate | |
---|---|---|---|---|---|---|
Scallion-flavored Soda Cake | ND | ND | ND | ND | ND | ND |
Rice noodles | ND | ND | ND | ND | ND | ND |
Osmanthus Lotus Root Cake | ND | ND | ND | ND | ND | ND |
Corn flour | 0.63 | 1.91 | 2.23 | 2.29 | ND | ND |
Pacific Soda Cake | ND | ND | ND | ND | ND | ND |
Evergreen Crispy Biscuit | 2.42 | 2.85 | 2.94 | 2.71 | ND | ND |
Sugar-free, high-fiber crispy biscuits | 2.40 | 1.92 | 1.90 | 1.76 | ND | ND |
Gangrong Steamed Cake | ND | ND | ND | ND | ND | ND |
Gangrong Steamed Bread | ND | ND | ND | ND | ND | ND |
Gangrong Sandwich Sandwich Cake | ND | ND | ND | ND | ND | ND |
Barbie Bear Pure Cake | ND | ND | ND | ND | ND | ND |
Barbie Bear Fresh Cake | ND | ND | ND | ND | ND | ND |
Hometown Sweet Pork Floss and Cheese Small Rolls | ND | ND | ND | ND | ND | ND |
Hometown Fruit Cake | ND | ND | ND | ND | ND | ND |
Hamburg cake | ND | ND | ND | ND | ND | ND |
White Peach Milk Cake | ND | ND | ND | ND | ND | ND |
Cheese milk cake | ND | ND | ND | ND | ND | ND |
Sucrose-free cake | ND | ND | ND | ND | ND | ND |
Sea salt cheese cake | ND | ND | ND | ND | ND | ND |
Milk vanilla-flavored small cake | ND | ND | ND | ND | ND | ND |
Honey cheese-flavored small cake | ND | ND | ND | ND | ND | ND |
Condensed milk toast | ND | ND | ND | ND | ND | ND |
Purple Rice Toast | ND | ND | ND | ND | ND | ND |
Cheese toast | ND | ND | ND | ND | ND | ND |
Yeast Salty Toast | ND | ND | ND | ND | ND | ND |
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Wang, L.; Hu, Z.; Chen, J.; Wang, T.; Wu, P.; Ying, Y. Simultaneous Determination of 12 Preservatives in Pastries Using Gas Chromatography–Mass Spectrometry. Foods 2023, 12, 3819. https://doi.org/10.3390/foods12203819
Wang L, Hu Z, Chen J, Wang T, Wu P, Ying Y. Simultaneous Determination of 12 Preservatives in Pastries Using Gas Chromatography–Mass Spectrometry. Foods. 2023; 12(20):3819. https://doi.org/10.3390/foods12203819
Chicago/Turabian StyleWang, Liyuan, Zhengyan Hu, Jing Chen, Tianjiao Wang, Pinggu Wu, and Ying Ying. 2023. "Simultaneous Determination of 12 Preservatives in Pastries Using Gas Chromatography–Mass Spectrometry" Foods 12, no. 20: 3819. https://doi.org/10.3390/foods12203819