Quality Control and Safety Assessment of Online-Purchased Food Supplements Containing Red Yeast Rice (RYR)
Abstract
:1. Introduction
2. Materials and Methods
2.1. Sample Set
2.2. Solvents, Reagents, and Standard Solutions
2.3. Targeted Screening Methodology for Natural Statins (Monacolins) and Synthetic Statins
2.4. Quantification of Citrinin and Monacolin K
2.5. Elemental Analyzer–Isotope Ratio Mass Spectrometry (EA-IRMS)
2.6. Bioburden Determination and Identification of the Encountered Micro-Organisms
2.7. Mycotoxin Determination
3. Results and Discussion
3.1. Food Supplement Labeling
3.2. Screening for Synthetic Statins
3.3. Citrinin, Total Monacolin K (MKtotal) Content, and Possible Adulteration
3.4. Bioburden, Identification of Micro-Organisms, and Mycotoxin Determination
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Retention Time (min) | Precursor Ion (m/z) | Fragment Ions (m/z) and Their Relative Intensities | Limit of Quantification (LLOQ) | Linear Range (LLOQ-ULOQ) | |
---|---|---|---|---|---|
citrinine | 3.4 | 251.091 [M + H]+ | 91.054 (100), 119.085 (50) | 5 ng/mL (20 ng/g food supplement) | 5–1000 ng/mL |
SIL-citrinine | 3.4 | 264.1339 [M + H]+ | 98.0781 (100), 128.1159 (70) | ||
MKA | 4.0 | 405.262 [M - H2O + H]+ | 199.148 (100), 173.132 (80) | 100 ng/mL (500 ng/g food supplement) | 100–5000 ng/mL |
D3-MKA | 4.0 | 408.282 [M - H2O + H]+ | 199.148 (100), 173.132 (90) | ||
MK | 4.5 | 405.262 [M - H2O + H]+ | 199.148 (100), 173.132 (75) | 50 ng/mL (250 ng/g food supplement) | 50–2000 ng/mL |
D3-MK | 4.5 | 408.282 [M - H2O + H]+ | 199.148 (90), 173.132 (100) |
Concentration Level | Recovery (%) | |||
---|---|---|---|---|
Citrinine | MKA | MK | ||
Matrix 1 | LLOQ | 93.2 | 104.4 | 96.5 |
ULOQ | 102.8 | 104.7 | 96.7 | |
Matrix 2 | LLOQ | 98.3 | 96.3 | 100.5 |
ULOQ | 97.5 | 97.9 | 98.4 | |
Matrix 3 | LLOQ | 92.6 | 91.5 | 98.5 |
ULOQ | 97.2 | 105.6 | 94.8 | |
Matrix 4 | LLOQ | n.a. | 94.5 | 103.7 |
ULOQ | n.a. | 98.6 | 95.6 |
Sample N° | Lot Number and Expiration Date Present | Warning on the Label a | Ingredients or Other API Declared on the Label | Maximum Serving Size According to Labeled Directions | Labeled Amount (mg) per Maximum Serving Size | Synthetic Statins Found in the Sample c | Amount of Citrinin Found (Mean ± MU, ng/g) | Measured Amount (mean ± MU, mg) per Maximum Serving MKtotal | |
---|---|---|---|---|---|---|---|---|---|
Total Monacolin | MKtotal b | ||||||||
1 | yes | n.a. | n.d. | 2 capsules | absent | absent | n.d. | 46.2 ± 0.3 | n.d. |
2 | yes | yes | Coenzyme Q10 and phytosterols | 3 capsules | n.d. | 2.8 | n.d. | n.d. | 2.36 ± 0.1 |
3 | yes | no | Leucine | 1 capsule | n.d. | 2.95 | n.d. | n.d. | 1.79 ± 0.02 |
4 | yes | yes | Coenzyme Q10, vitamin E, vitamin C, niacin, plant extracts (sage, garlic, Astragalus, sugar cane) | 1 capsule | n.d. | 2.54 | n.d. | n.d. | 1.19 ± 0.03 |
5 | yes | yes | Coenzyme Q10, vitamin B6, plant extracts (Silybum and Filipendula) | 1 capsule | n.d. | 2.9 | n.d. | n.d. | 1.54 ± 0.03 |
6 | yes | no | n.d. | 1 capsule | n.d. | 2.9 | n.d. | n.d. | 2.78 ± 0.12 |
7 | yes | yes | Leucine | 1 capsule | n.d. | 2.95 | n.d. | n.d. | 2.57 ± 0.04 |
8 | yes | yes | n.d. | 1 capsule | n.d. | 1.0 | n.d. | 40.5 ± 0.6 | 1.15 ± 0.04 |
9 | yes | yes | Coenzyme Q10, vitamin B3 | 1 tablet | n.d. | 2.9 | n.d. | n.d. | 2.15 ± 0.06 |
10 | yes | n.a. | n.d. | 2 tablets | n.d. | n.d. | n.d. | 58.7 ± 0.3 | n.d. |
11 | yes | n.a. | Coenzyme Q10 | 2 soft gels | n.d. | n.d. | n.d. | <20 | n.d. |
12 | yes | yes | Vitamin B1 | 1 capsule | n.d. | 2.9 | n.d. | n.d. | 1.13 ± 0.02 |
13 | no | no | n.d. | 2 capsules | n.d. | n.d. | n.d. | n.d. | n.d. |
14 | yes | no | Coenzyme Q10 | 2 capsules | 2.4 | n.d. | n.d. | <20 | 3.51 ± 0.06 |
15 | yes | no | n.d. | 2 capsules | n.d. | absent | n.d. | 23.8 ± 0.1 | n.d. |
16 | yes | no | n.d. | 2 capsules | n.d. | absent | n.d. | 24.0 ± 0.04 | n.d. |
17 | yes | yes | n.d. | 1 capsule | 2.9 | n.d. | n.d. | <20 | 2.66 ± 0.02 |
18 | yes | yes | n.d. | 1 tablet | 2.99 | n.d. | n.d. | <20 | 4.25 ± 0.24 |
19 | yes | yes | Folic acid, coenzyme Q10, berberine | 1 tablet | 2.8 | n.d. | n.d. | n.d. | 1.84 ± 0.05 |
20 | yes | yes | Coenzyme Q10, folic acid, vitamin B12, plant extract (Coriandrum sativum) | 1 tablet | 2.9 | n.d. | n.d. | 41.9 ± 0.2 | 1.97 ± 0.05 |
21 | yes | yes | Coenzyme Q10, different plant extracts (Allium sativum and Olea europeae) | 2 liquid capsules | 2.99 | n.d. | n.d. | 21.4 ± 0.1 | 1.52 ± 0.02 |
22 | yes | yes | Coenzyme Q10, different plant extracts (Allium sativum and Olea europeae) | 2 capsules | 2.99 | n.d. | n.d. | n.d. | 1.31 ± 0.05 |
23 | yes | yes | n.d. | 1 capsule | 2.9 | n.d. | n.d. | n.d. | 1.41 ± 0.04 |
24 | yes | yes | Coenzyme Q10 and berberine | 2 capsules | 2.99 | n.d. | n.d. | n.d. | 3.19 ± 0.2 |
25 | yes | yes | Vitamin B1, plant extracts (Cynara scolymus and Olea europeae) | 1 tablet | 2.9 | n.d. | n.d. | n.d. | 1.30 ± 0.15 |
26 | yes | yes | Plant extracts (Cynara scolymus and Olea europeae) | 1 tablet | 2.95 | n.d. | n.d. | n.d. | 1.25 ± 0.03 |
27 | yes | yes | Coenzyme Q10, cinnamon and green tea extract | ½ tablet | 2.885 | 1.9 | n.d. | 33.6 ± 0.2 | 0.81 ± 0.01 |
28 | yes | yes | Vitamin B3, vitamin E, and coenzyme Q10 | 1 tablet | n.d. | 2.99 | n.d. | n.d. | 1.58 ± 0.03 |
29 | yes | yes | n.d. | 1 tablet | 2.5 | n.d. | n.d. | 38.7 ± 0.1 | 2.31 ± 0.07 |
30 | yes | yes | Vitamin B1 | 1 tablet | 2.9 | n.d. | n.d. | <20 | 1.83 ± 0.07 |
31 | yes | yes | Ascorbic acid, vitamin B1, different plant extracts (sage, Coriandrum sativum, and Tinospora cordifolia) | 2 capsules | n.d. | 1.48 | n.d. | n.d | 6.13 ± 0.12 |
32 | yes | yes | n.d. | 1 capsule | 2.95 | n.d. | n.d. | n.d | 2.71 ± 0.04 |
33 | yes | yes | Plant extract (Allium sativum and Cynara scolymus) | 1 capsule | 2.99 | n.d. | n.d. | n.d. | 0.99 ± 0.03 |
34 | yes | yes | n.d. | 1 capsule | n.d. | 2.95 | n.d. | <20 | 2.53 ± 0.09 |
35 | yes | yes | n.d. | 1 capsule | n.d. | 2.9 | n.d. | <20 | 2.34 ± 0.04 |
Sample N° | Amount Found per Maximum Serving Size (mean ± MU, mg) | Ratio MKA/MKtotal | δ13 C Values of MK (‰) | ||
---|---|---|---|---|---|
MKA | MK | MKtotal | |||
2 | 0.70 (±0.03) | 1.66 (±0.02) | 2.36 (±0.09) | 0.30 | n.a. |
3 | 1.35 (±0.03) | 0.44 (±0.02) | 1.79 (±0.03) | 0.75 | n.a. |
4 | 0.15 (±0.01) | 1.04 (±0.03) | 1.19 (±0.03) | 0.13 | −17.6 |
5 | 0.70 (±0.03) | 0.84 (±0.01) | 1.54 (±0.03) | 0.45 | n.a. |
6 | 2.17 (±0.12) | 0.61 (±0.003) | 2.78 (±0.12) | 0.78 | n.a. |
7 | 1.95 (±0.03) | 0.61 (±0.03) | 2.56 (±0.04) | 0.76 | n.a. |
8 | 0.18 (±0.01) | 0.96 (±0.03) | 1.15 (±0.04) | 0.16 | −30.1 |
9 | 0.88 (±0.02) | 1.26 (±0.03) | 2.15 (±0.06) | 0.41 | n.a. |
12 | 0.56 (±0.03) | 0.58 (±0.01) | 1.13 (±0.02) | 0.49 | n.a. |
14 | 0.99 (±0.02) | 2.52 (±0.05) | 3.51 (±0.06) | 0.28 | −28.5 |
17 | 0.63 (±0.01) | 2.02 (±0.02) | 2.66 (±0.02) | 0.24 | −28.1 |
18 | 3.67 (±0.25) | 0.58 (±0.01) | 4.25 (±0.24) | 0.86 | n.a. |
19 | 1.23 (±0.03) | 0.61 (±0.02) | 1.84 (±0.05) | 0.67 | n.a. |
20 | 0.23 (±0.01) | 1.73 (±0.05) | 1.97 (±0.05) | 0.12 | −29.6 |
21 | 0.41 (±0.02) | 1.11 (±0.03) | 1.52 (±0.02) | 0.27 | n.d. |
22 | 0.43 (±0.03) | 0.88 (±0.01) | 1.31 (±0.05) | 0.33 | n.a. |
23 | 0.42 (±0.04) | 0.99 (±0.02) | 1.41 (±0.04) | 0.30 | n.a. |
24 | 1.15 (±0.05) | 2.03 (±0.03) | 3.19 (±0.20) | 0.36 | n.a. |
25 | 0.51 (±0.01) | 0.79 (±0.02) | 1.3 (±0.02) | 0.39 | n.a. |
26 | 0.35 (±0.03) | 0.91 (±0.04) | 1.25 (±0.03) | 0.28 | −22.6 |
27 | 0.44 (±0.02) | 0.37 (±0.01) | 0.81 (±0.01) | 0.54 | n.a. |
28 | 1.04 (±0.05) | 0.54 (±0.02) | 1.58 (±0.03) | 0.66 | n.a. |
29 | 0.72 (±0.03) | 1.58 (±0.06) | 2.3 (±0.07) | 0.31 | n.a. |
30 | 0.93 (±0.01) | 0.90 (±0.02) | 1.83 (±0.07) | 0.51 | n.a. |
31 | 5.97 (±0.06) | 0.16 (±0.004) | 6.13 (±0.12) | 0.97 | n.a. |
32 | 0.39 (±0.01) | 2.31 (±0.05) | 2.7 (±0.04) | 0.14 | −30.0 |
33 | 0.22 (±0.02) | 0.77 (±0.04) | 0.99 (±0.03) | 0.22 | −25.0 |
34 | 0.56 (±0.03) | 1.96 (±0.12) | 2.52 (±0.09) | 0.22 | −30.4 |
35 | 0.56 (±0.03) | 1.78 (±0.06) | 2.34 (±0.04) | 0.24 | −30.2 |
Sample N° | TAMC | Growth on Bile Acid Medium (CFU/g or mL) | TYMC | ||
---|---|---|---|---|---|
CFU/g or mL | Identified Organism | CFU/g or mL | Identified Organism | ||
1 | n.d. | n.d. | n.d. | n.d. | n.d. |
2 | 2.5 × 103 | Bacillus velenzis | n.d. | n.d. | n.d. |
3 | n.d. | n.d. | n.d. | 50 | Penicillium olsonii |
4 | 2 × 103 | Bacillus velenzis and Bacillus spp. | n.d. | n.d. | n.d. |
5 | 2.5 × 102 | Bacillus velenzis | n.d. | 50 | Aspergillus niger |
6 | 1 × 103 | Bacillus spp. | n.d. | n.d. | n.d. |
7 | n.d. | n.d. | n.d. | n.d. | n.d. |
8 | n.d. | n.d. | n.d. | n.d. | n.d. |
9 | n.d. | n.d. | n.d. | n.d. | n.d. |
10 | 2 × 102 | Bacillus subtilis | n.d. | n.d. | n.d. |
11 | n.d. | n.d. | n.d. | n.d. | n.d. |
12 | n.d. | n.d. | n.d. | n.d. | n.d. |
13 | 1.5 × 102 | Roseomonas mucosa | n.d. | n.d. | n.d. |
14 | 3.5 × 104 | Bacillus subtilis | n.d. | n.d. | n.d. |
15 | n.d. | n.d. | n.d. | n.d. | n.d. |
16 | 3 × 102 | Kocuria rhizophila | n.d. | n.d. | n.d. |
17 | 1.5 × 103 | Bacillus spp. and Staphylococcus capitis | n.d. | n.d. | n.d. |
18 | n.d. | n.d. | n.d. | n.d. | n.d. |
19 | n.d. | n.d. | n.d. | n.d. | n.d. |
20 | 4 × 102 | Bacillus cereus | n.d. | n.d. | n.d. |
21 | n.d. | n.d. | n.d. | n.d. | n.d. |
22 | 2 × 102 | Bacillus amyloliquifaciens | n.d. | n.d. | n.d. |
23 | n.d. | n.d. | n.d. | n.d. | n.d. |
24 | n.d. | n.d. | n.d. | n.d. | n.d. |
25 | n.d. | n.d. | n.d. | n.d. | n.d. |
26 | n.d. | n.d. | n.d. | n.d. | n.d. |
27 | 50 | Niallia taxi | n.d. | n.d. | n.d. |
28 | n.d. | n.d. | n.d. | n.d. | n.d. |
29 | 2.5 × 103 | Acinetobacter johnsonii | 2.5 × 103 | 150 | Cladosporium uwebraunianum |
30 | n.d. | n.d. | n.d. | n.d. | n.d. |
31 | n.d. | n.d. | n.d. | n.d. | n.d. |
32 | n.d. | n.d. | n.d. | n.d. | n.d. |
33 | n.d. | n.d. | n.d. | 75 | Penicillium rubens |
34 | 1 × 102 | Bacillus spp. | n.d. | n.d. | n.d. |
35 | n.d. | n.d. | n.d. | n.d. | n.d. |
Sample N° | Mycotoxin Concentration (ng/g) | |||||
---|---|---|---|---|---|---|
AF | OTA | T2 + HT2 | DON | FB1–3 | ZEN | |
1 | n.d. | n.d. | n.d. | n.d. | n.d. | 96.70 |
5 | n.d. | 5.82 | 724.09 | 288.25 | <10 | n.d. |
6 | n.d. | n.d. | n.d. | 412.35 | n.d. | n.d. |
7 | n.d. | n.d. | n.d. | 28.05 | <10 | n.d. |
10 | n.d. | n.d. | n.d. | n.d. | n.d. | 29.06 |
11 | n.d. | n.d. | n.d. | n.d. | n.d. | 25.90 |
13 | n.d. | n.d. | n.d. | n.d. | n.d. | 16.95 |
14 | <1 | n.d. | n.d. | n.d. | 17.72 | n.d. |
16 | n.d. | n.d. | n.d. | n.d. | n.d. | 65.19 |
21 | n.d. | n.d. | n.d. | n.d. | 32.23 | n.d. |
33 | n.d. | n.d. | n.d. | 51.57 | 17.75 | n.d. |
35 | <1 | n.d. | n.d. | n.d. | 17.41 | n.d. |
Max. limit (ng/g) | 4 a | 15 b | - | - | - | - |
TDI (ng/kg bw) | - | - | 20 | 1000 | 2000 | 250 |
ADI (ng) | - | - | 1200 | 60,000 | 120,000 | 15,000 |
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Vanhee, C.; Jacobs, B.; Canfyn, M.; Malysheva, S.V.; Willocx, M.; Masquelier, J.; Van Hoorde, K. Quality Control and Safety Assessment of Online-Purchased Food Supplements Containing Red Yeast Rice (RYR). Foods 2024, 13, 1919. https://doi.org/10.3390/foods13121919
Vanhee C, Jacobs B, Canfyn M, Malysheva SV, Willocx M, Masquelier J, Van Hoorde K. Quality Control and Safety Assessment of Online-Purchased Food Supplements Containing Red Yeast Rice (RYR). Foods. 2024; 13(12):1919. https://doi.org/10.3390/foods13121919
Chicago/Turabian StyleVanhee, Celine, Bram Jacobs, Michael Canfyn, Svetlana V. Malysheva, Marie Willocx, Julien Masquelier, and Koenraad Van Hoorde. 2024. "Quality Control and Safety Assessment of Online-Purchased Food Supplements Containing Red Yeast Rice (RYR)" Foods 13, no. 12: 1919. https://doi.org/10.3390/foods13121919