Microbiological and Chemical Quality of Portuguese Lettuce—Results of a Case Study
Abstract
:1. Introduction
2. Materials and Methods
2.1. Sampling
2.2. Microbiological Analysis
2.3. Chemical Safety Analysis
2.3.1. Chemicals, Materials and Standards
2.3.2. Nitrate Concentration
2.3.3. Pesticides Determination
Sample Preparation
Method Validation
GC Analysis
2.4. Statistical Analyses
3. Results and Discussion
3.1. Microbiological Analysis
3.2. Nitrate Concentration
3.3. Pesticide Analysis
3.3.1. Method Evaluation
3.3.2. Sample Analysis
4. Conclusions
Author Contributions
Funding
Conflicts of Interest
References
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GC-ECD | GC-FPD | GC/MS | |
---|---|---|---|
Equipment | Shimadzu GC-2010 gas chromatograph (Shimadzu, Kyoto, Japan) | Shimadzu GC-2010 Plus gas chromatograph (Shimadzu, Kyoto, Japan) | Thermo Trace-Ultra GC from Thermo Fisher Scientific (Waltham, MA, USA) coupled to an ion trap mass detector Thermo Polaris |
Column | Zebron-5MS, 30 m × 0.25 mm, 0.25 µm film | ||
Carrier Gas | Helium at 1 mL min−1 | ||
Injection | 2 µL splitless | ||
Temperature: Injector Detector | 250 °C | 250 °C | 250 °C |
300 °C | 290 °C | Transfer line 250 °C/Ion source 270 °C | |
Temperature program | Initial 40 °C, hold 1 min, then 20 °C/min to 120 °C, hold 1 min, next 10 °C/min to 150 °C, hold 1 min, next 10 °C/min to 180 °C, hold 1 min, next 20 °C/min to 200 °C, hold 1 min, next 10 °C/min to 290 °C and hold 2 min. | Initial 100 °C, hold 1 min, then 20 °C/min to 150 °C, hold 1 min, next 2 °C/min to 180 °C, hold 2 min, and 20 °C/min to 270 °C and hold for 1 min. | Same as ECD |
Total running time | 27 min | 26 min | 27 min |
Others: | SIM mode confirmation α-HCH | m/z 109, 181, 219 |
Log (CFU/g) | |||||||
---|---|---|---|---|---|---|---|
Production Mode | Sample | Enterobacteria | Total Counts | Lactic Acid Bacteria | Pseudomonas Spp. | Molds | Yeasts |
Conventional | Conv1 | 6.5 | 8.0 | 3.4 | 7.7 | 4.3 | 6.0 |
Conv2 | 4.3 | 8.3 | 4.2 | 7.4 | 4.6 | 7.2 | |
Conv3 | 7.1 | 7.8 | 3.4 | 1 | 4.5 | 5.3 | |
Conv4 | 4.9 | 8.0 | 3.2 | 6.4 | 4.8 | 5.6 | |
Conv5 | 5.1 | 8.3 | 7.3 | 7.3 | 5.2 | 5.9 | |
Conv6 | 7.0 | 8.9 | 3.9 | 7.4 | 5.1 | 5.5 | |
Conv7 | 4.9 | 8.5 | * | 7.0 | 4.4 | 7.1 | |
Conv8 | 6.4 | 9.2 | 4.2 | 7.1 | 4.2 | 6.4 | |
Conv9 | 6.0 | 9.2 | 4.0 | 6.6 | 5.4 | 7.0 | |
Conv10 | 6.8 | 7.8 | 1.0 | 6.1 | 4.9 | 5.8 | |
Average ± SD | 5.9 ± 1.0 | b 8.4 ± 0.54 | 3.8 ± 1.6 | 6.4 ± 2.0 | 4.7 ± 0.41 | 6.2 ± 0.7 | |
Organic | Org1 | 4.7 | 7.8 | 3.4 | 7.6 | 3.4 | 4.3 |
Org2 | <1 | 7.2 | 3.5 | 3.7 | 4.6 | 5.2 | |
Org3 | 6.4 | 7.5 | 2.7 | 7.5 | 5.4 | 6.1 | |
Org4 | 3.0 | 7.4 | 1.0 | 7.2 | 4.9 | 9.2 | |
Org5 | 4.1 | 6.1 | 1.0 | 6.0 | 2.2 | 4.5 | |
a Org6 | 7.5 | 8.9 | 3.3 | 7.3 | 5.5 | 6.3 | |
a Org7 | 4.3 | 7.4 | 3.6 | 6.6 | 5.0 | 5.6 | |
a Org8 | 6.7 | 7.4 | 3.3 | 6.9 | 5.3 | 6.3 | |
Org9 | 6.1 | 8.0 | * | 7.4 | 4.5 | 6.7 | |
Org10 | 6.9 | 8.1 | 1.0 | 6.8 | 5.4 | 6.4 | |
Average ± SD | 5.2 ± 1.5 | b 7.6 ± 0.72 | 2.5 ± 1.2 | 6.7 ± 1.2 | 4.6 ± 1.1 | 6.1 ± 1.4 |
Production Mode | |||
---|---|---|---|
Conventional | Organic | ||
Sample | Nitrate (mg/kg) | Sample | Nitrate (mg/kg) |
Conv1 | 1290 | Org1 | 1550 |
Conv2 | 1760 | Org2 | 1530 |
Conv3 | 1650 | Org3 | 1720 |
Conv4 | 1590 | Org4 | 1670 |
Conv5 | 1630 | Org5 | 1410 |
Conv6 | * | a Org6 | 1580 |
Conv7 | * | a Org7 | 1610 |
Conv8 | 1950 | a Org8 | * |
Conv9 | 1370 | Org9 | 1480 |
Conv10 | 1606 | Org10 | 1569 |
Average ± SD | 1606 ± 207 | 1569 ± 93 |
Recoveries ± Relative Standard Deviation (RSD) (%) (n = 3) | |||||||
---|---|---|---|---|---|---|---|
Analytes | MRL * µg/kg | Coefficient of Determination | LOQ µg/kg | 25 µg/kg | 50 µg/kg | 100 µg/kg | |
Organophosphorus pesticides | Diazinon | 10 | 0.9956 | 1.13 | 78 ± 15 | 81 ± 18 | 85 ± 17 |
Chlorpyrifos-methyl | 10 | 0.9929 | 1.57 | 70 ± 12 | 84 ± 10 | 83 ± 13 | |
Parathion-methyl | 10 | 0.9989 | 0.57 | 74 ± 17 | 95 ± 9 | 80 ± 15 | |
Malathion | 500 | 0.9982 | 0.72 | 55 ± 20 | 60 ± 10 | 65 ± 14 | |
Chlorpyrifos | 10 | 0.9963 | 1.03 | 79 ± 10 | 87 ± 17 | 90 ± 16 | |
Chlorfenvinphos | 10 | 0.9956 | 1.13 | 71 ± 16 | 83 ± 10 | 79 ± 9 | |
Organochlorine pesticides | α-HCH | 10 | 0.9980 | 0.77 | 85 ± 16 | 90 ± 8 | 87 ± 18 |
HCB | 10 | 0.9927 | 1.46 | 90 ± 15 | 95 ± 15 | 90 ± 9 | |
β-HCH | 10 | 0.9960 | 1.08 | 78 ± 11 | 84 ± 10 | 80 ± 12 | |
lindane (γ-HCH) | 10 | 0.9944 | 1.11 | 89 ± 20 | 97 ± 11 | 90 ± 14 | |
ζ-HCH | 10 | 0.9900 | 1.49 | 75 ± 8 | 82 ± 8 | 80 ± 1 | |
Aldrin | 10 | 0.9976 | 0.73 | 79 ± 7 | 84 ± 7 | 79 ± 7 | |
Endosulfan I | 50 | 0.9943 | 1.12 | 80 ± 2 | 89 ± 5 | 85 ± 4 | |
p.p’-DDE | 50 | 0.9932 | 1.13 | 81 ± 2 | 92 ± 5 | 90 ± 1 | |
Dieldrin | 10 | 0.9979 | 0.80 | 90 ± 5 | 94 ± 11 | 90 ± 9 | |
Endrin | 10 | 0.9925 | 1.79 | 78 ± 5 | 86 ± 8 | 82 ± 4 | |
DDT # | 50 | 0.9958 | 0.96 | 72 ± 6 | 81 ± 10 | 80 ± 5 | |
p.p′-DDD | 50 | 0.9913 | 1.59 | 75 ± 19 | 82 ± 11 | 78 ± 11 | |
Endosulfan II | 50 | 0.9956 | 0.79 | 82 ± 2 | 90 ± 9 | 86 ± 1 | |
Methoxychlor | 0.9994 | 0.78 | 73 ± 2 | 80 ± 7 | 79 ± 3 |
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Share and Cite
Ferreira, C.; Lopes, F.; Costa, R.; Komora, N.; Ferreira, V.; Cruz Fernandes, V.; Delerue-Matos, C.; Teixeira, P. Microbiological and Chemical Quality of Portuguese Lettuce—Results of a Case Study. Foods 2020, 9, 1274. https://doi.org/10.3390/foods9091274
Ferreira C, Lopes F, Costa R, Komora N, Ferreira V, Cruz Fernandes V, Delerue-Matos C, Teixeira P. Microbiological and Chemical Quality of Portuguese Lettuce—Results of a Case Study. Foods. 2020; 9(9):1274. https://doi.org/10.3390/foods9091274
Chicago/Turabian StyleFerreira, Catarina, Filipa Lopes, Reginaldo Costa, Norton Komora, Vânia Ferreira, Virgínia Cruz Fernandes, Cristina Delerue-Matos, and Paula Teixeira. 2020. "Microbiological and Chemical Quality of Portuguese Lettuce—Results of a Case Study" Foods 9, no. 9: 1274. https://doi.org/10.3390/foods9091274