Source: https://patents.justia.com/patent/10267810
Timestamp: 2019-10-23 12:36:33
Document Index: 108261128

Matched Legal Cases: ['Application No. 2013', 'Application No. 06749272', 'Application No. 08853843', 'Application No. 10836702', 'Application No. 10836711', 'Application No. 11184151', 'Application No. 16154623']

US Patent for Methods for detecting vitamin D metabolites by mass spectrometry Patent (Patent # 10,267,810 issued April 23, 2019) - Justia Patents Search
Justia Patents Hydroxyl ContainingUS Patent for Methods for detecting vitamin D metabolites by mass spectrometry Patent (Patent # 10,267,810)
Dec 20, 2017 - Quest Diagnostics Investments Incorporated
Provided are methods of detecting the presence or amount of a vitamin D metabolite in a sample using mass spectrometry. The methods generally directed to ionizing a vitamin D metabolite in a sample and detecting the amount of the ion to determine the presence or amount of the vitamin D metabolite in the sample. Also provided are methods to detect the presence or amount of two or more vitamin D metabolites in a single assay.
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This application is a continuation of U.S. application Ser. No. 15/388,844, filed Dec. 22, 2016, now U.S. Pat. No. 9,880,180, which is a continuation of U.S. application Ser. No. 15/005,801, filed Jan. 25, 2016, now U.S. Pat. No. 9,529,004, which is a continuation of U.S. application Ser. No. 14/180,722, filed Feb. 14, 2014, now U.S. Pat. No. 9,244,084, which is a continuation of U.S. application Ser. No. 13/871,457, now U.S. Pat. No. 8,936,943, filed Apr. 26, 2013, which is a continuation of U.S. application Ser. No. 13/327,650, now U.S. Pat. No. 8,431,411, filed Dec. 15, 2011, which is a continuation of U.S. application Ser. No. 13/115,916, now U.S. Pat. No. 8,101,427, filed May 25, 2011, which is a continuation of U.S. application Ser. No. 11/386,215, now U.S. Pat. No. 7,972,867, filed Mar. 21, 2006, which is a continuation-in-part of U.S. application Ser. No. 11/101,166, now U.S. Pat. No. 7,745,226, filed Apr. 6, 2005, each of which is incorporated by reference in its entirety herein.
EXAMPLES Example 1: Determination of 25-hydroxyvitamin D3 and 25-hydroxyvitamin D2 by LC-MS/MS
Example 2: Intra-Assay and Inter-Assay Precision
Example 3: Analytical Sensitivity: Limit of Detection and Limit of Quantitation Studies
0 ng/mL −1.2 −1.3 −0.5 −1.2 −1.1 Average (ng/mL) −1.0 −1.1 −1.4 −0.9 −1.3 −0.7 Standard Deviation 0.6 −1.1 −1.5 −0.8 NA −2.6 C of V (%) 59.0 0.4 −1.7 −0.6 −0.5 −0.6 Accuracy (%) N/A 2 ng/mL 3.1 2.3 2.0 2.1 3.3 Average (ng/mL) 1.9 2.1 2.7 2.1 2.4 1.9 Standard Deviation 0.6 1.1 1.9 1.9 0.9 1.3 C of V (%) 33.7 1.2 1.1 2.1 1.8 1.4 Accuracy (%) 103.9 4 ng/mL 3.5 3.9 5.0 4.5 4.8 Average (ng/mL) 3.9 4.0 3.0 3.8 3.8 4.7 Standard Deviation 0.7 3.6 2.9 2.8 3.1 2.0* C of V (%) 17.1 4.1 4.6 4.5 4.4 3.7 Accuracy (%) 101.7 8 ng/mL 10.2 9.1 9.1 8.8 9.8 Average (ng/mL) 8.6 7.8 8.1 7.9 8.4 9.0 Standard Deviation 0.8 8.6 8.3 7.4 8.4 7.5 C of V (%) 9.3 10.2 8.4 8.0 8.1 8.6 Accuracy (%) 93.2 16 ng/mL 16.0 14.8 14.4 16.7 18.3 Average (ng/mL) 16.0 15.5 15.6 15.3 16.7 16.8 Standard Deviation 1.1 16.6 16.7 16.8 15.8 15.2 C of V (%) 7.1 14.1 17.6 16.1 16.7 14.1 Accuracy (%) 100.1 32 ng/mL 31.3 39.9* 29.9 33.2 32.7 Average (ng/mL) 31.8 31.7 30.5 32.4 34.0 32.5 Standard Deviation 1.9 29.5 31.2 30.2 35.7 28.7 C of V (%) 6.0 32.9 34.7 32.4 30.8 29.2 Accuracy (%) 100.7 64 ng/mL 66.5 62.2 68.5 62.6 68.8 Average (ng/mL) 64.6 66.6 67.8 67.3 58.9 61.5 Standard Deviation 3.2 64.4 61.4 63.7 63.5 61.3 C of V (%) 4.9 63.7 60.7 65.4 70.8 65.9 Accuracy (%) 99.1 128 ng/mL 125.1 128.2 123.4 127.8 124.1 Average (ng/mL) 126.9 127.6 134.4 127.3 128.4 132.1 Standard Deviation 3.5 128.9 124.5 128.5 126.5 131.7 C of V (%) 2.8 126.1 119.7 127.9 121.2 125.0 Accuracy (%) 100.8
Day #1 Day #2 Day #3 Day #4 Day #5 (Nov. 19, (Nov. 19, (Nov. 22, (Nov. 23, (Nov. 23, 2004-1) 2004-2) 2004-1) 2004-1) 2004-2) Summary
Example 4: Assay Reportable Range and Linearity
Additionally, solutions of 25OHD2 and 25OHD3 at 512 ng/mL in 5% Bovine Serum Albumin Fraction V dissolved in 0.01M PBS were prepared and then serially diluted to 8 ng/mL. Each sample was extracted and run in duplicate using the LC-MS/MS protocols described in Example 1. As shown in FIG. 3, each of these curves was linear (R2>0.99).
Example 5: Accuracy of LC-MS/MS Vitamin D Assay
Example 6: Comparison LC-MS/MS Vitamin D Metabolite Assay and RIA Procedures
Example 7: Selectivity of the LC-MS/MS Assay
25-Hydroxyvitamin D2 412 (100%) ND (25OHD2) 25-Hydroxyvitamin D3 400 ND (100%) (25OHD3) Internal Standard (6D-25OHD3) 406 ND ND Vitamin D2 (Ergocalciferol) 396 ND ND Vitamin D3 (Cholecalciferol) 384 ND ND 1α,25(OH)2D2 428 ND ND 1α,25(OH)2D3 416 ND ND 25,26(OH)2D3 416 ND ND 1α(OH)D2 (Doxercalciferol) 412 ND ND 1α(OH)D3 (Alfacalcidiol) 400 ND ND
(a) generating a protonated and dehydrated precursor ion of said vitamin D metabolite by atmospheric pressure chemical ionization (APCI);
(c) detecting the amount of one or more of said ions generated in step (a) or (b) or both and relating the detected ions to the presence or amount of said vitamin D metabolite in said sample;
wherein said vitamin D metabolite is 25-hydroxyvitamin D3 or 25-hydroxyvitamin D2.
2. The method of claim 1, wherein said sample is subjected to a purification step prior to ionization step (a).
3. The method of claim 2, wherein said purification step comprises liquid chromatography.
4. The method of claim 3, wherein said liquid chromatography comprises high performance liquid chromatography (HPLC).
8. The method of claim 1, wherein said vitamin D metabolite is 25-hydroxyvitamin D3.
9. The method of claim 1, wherein said vitamin D metabolite is 25-hydroxyvitamin D2.
10. A method for determining the amount of 25-hydroxyvitamin D3 and 25-hydroxyvitamin D2 in a sample in a single assay, said method comprising:
(a) ionizing by atmospheric pressure chemical ionization (APCI) said 25-hydroxyvitamin D3 and 25-hydroxyvitamin D2 to generate protonated and dehydrated precursor ions specific for each of said 25-hydroxyvitamin D3 and 25-hydroxyvitamin D2;
(c) detecting the amount of one or more of said ions generated in step (a) or (b) or both and relating the detected ions to the amount of 25-hydroxyvitamin D3 and 25-hydroxyvitamin D2 in said sample.
11. The method of claim 10, wherein said sample subjected to a purification step prior to said ionization step (a).
12. The method of claim 11, wherein said purification step comprises liquid chromatography.
13. The method of claim 12, wherein said liquid chromatography comprises high performance liquid chromatography (HPLC).
14. The method of claim 11, wherein said purification step comprises protein precipitation and does not include high turbulence liquid chromatography.
15. The method of claim 10, wherein said sample comprises a biological sample.
16. The method of claim 10, wherein said sample comprises plasma or serum.
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Patent number: 10267810
Patent Publication Number: 20180156828
Inventors: Nigel J. Clarke (Vista, CA), Brett Holmquist (Mission Viejo, CA), Gloria Kwang-Ja Lee (Irvine, CA), Richard E. Reitz (Las Vegas, NV)
Application Number: 15/848,325
International Classification: G01N 33/82 (20060101); G01N 30/72 (20060101); G01N 30/88 (20060101); H01J 49/00 (20060101); H01L 49/00 (20060101);