AOAC SPIFAN ERP Meeting Book-March 16, 2016

Bio-02 w/SLV FOR ERP USE ONLY DO NOT DISTRIBUTE

Table 4: Repeatability

Biotin (µg/100g)

SPIFAN SLV Samples

RSD

Day 1

Day 2

Day 3

Day 4

Day 5

Day 6

Average

CLC10-b 197.42 201.01 196.08 196.28 197.93 201.54 198.54 198.39 199.34 198.81 197.00 197.30 198.30 0.86 11750017V3 12.77 12.73 12.67 12.77 12.69 12.69 12.53 12.73 12.61 12.62 12.65 12.70 12.68 0.55 1172572116 34.68 34.50 34.20 35.24 35.17 35.13 36.05 35.09 36.19 36.97 35.19 35.02 35.29 2.19 117257651Z 39.76 39.99 39.98 39.16 40.12 40.50 39.37 40.77 40.87 40.96 39.50 40.70 40.14 1.54 00394RF00 248.67 249.85 254.88 237.61 258.75 261.19 256.65 259.83 255.74 259.20 254.28 256.30 254.41 2.55 00412RF00 91.08 90.66 88.99 89.01 89.70 91.71 89.92 90.81 89.56 90.20 90.69 90.72 90.25 0.93 00403RF00 69.17 69.30 70.41 69.88 71.88 72.28 71.35 71.45 72.14 71.83 70.52 71.03 70.94 1.52 D04HTCVV 35.48 35.24 34.23 33.92 33.36 34.28 33.01 33.17 32.94 32.96 31.71 32.94 33.60 3.19 E29JVLV 43.30 43.25 45.40 44.72 45.02 44.38 45.29 44.85 45.15 44.78 44.76 45.08 44.67 1.58 Control Milk F 5.45 5.47 5.36 5.34 5.40 5.44 5.38 5.43 5.20 5.31 5.15 5.37 5.36 1.83 00414RF00 54.02 55.42 55.50 55.16 52.36 52.07 53.67 53.78 53.23 53.91 55.48 54.21 54.07 2.16 00406RF00 68.88 65.17 63.77 64.85 66.78 67.48 65.51 66.54 65.64 65.36 63.92 62.13 65.50 2.74 SRM 1849a 198.46 0.63 199.97 199.65 196.50 197.87 198.37 198.42 AsureQuality Auckland Laboratory has initiated a method to facilitate a specific, precise, accurate and robust procedure for the analysis of biotin from Infant Formula and Adult / Pediatric Nutritional Formulas. The method involves immunoaffinity column (R-Biopharm Rhone, EASI-EXTRACT biotin column) clean-up and extraction followed by liquid chromatography with UV detection. The proposed method exceeds all the SPIFAN SMPR for biotin. The method also has an assured limit of quantification of 0.1µg/100g (1ppb) based on a simple mathematical relationship between lowest standard and dilution. This method is found to be suitable for routine testing of biotin in infant formula and adult nutritionals. Comparison of SMPR for biotin and the proposed method performance are given in Table 5. 6. SUMMARY AND CONCLUSION

Table 5: Performance of the proposed method (Bio -02) compared to SMPR 2014.005 Parameters SMPR 2014.005 Proposed Method Comments

Analytical range of the proposed method is wider based on the sample weight taken and loading volume for sample extraction. The proposed method meets the LOQ of 0.1 µg/100g as required by AOAC SMPR 2014.005.

Analytical Range

0.1 - 150 µg/100g

0.1 - 300 µg/100g

Limit of Quantitation

≤ 0.1 µg/100g

≤ 0.1 µg/100g

Repeatability of the proposed method is better than the SMPR 2014.005.

Repeatability (RSD r )

>1 µg/100g: ≤ 6%

>1 µg/100g: ≤ 4%

All the spiked recoveries by the proposed method are better than the recovery range specified by AOAC SMPR 2014.005.

Recovery (>1µg/100g)

90 to 110%

95 to 105%

NIST 1949a results are at the certified value.

NIST SRM 1849a

199 ± 13

198 ± 3

5841 v2

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