1. Control Charting Mississippi Style ASHLI BROWN, GALE HAGOOD, DONGPING JIANG MISSISSIPPI STATE CHEMICAL LABORATORY GOVERNMENTAL FOOD AND FEED LABORATORIES ACCREDITATION MEETING FEBRUARY 2016

2. 5.9 Assuring the quality of Test and calibration results  5.9.1 The laboratory shall have quality control procedures for monitoring the validity of tests and calibrations undertaken. The resulting data shall be recorded in such a way that trends are detectable a) regular use of certified reference materials b) participation in interlaboratory comparison or proficiency-testing programs. QM-001 5.9.1 Quality Control Policy and Procedure: Quality control procedures are utilized to monitor the validity of test results. QP-026 defines the specific QC procedures used.  5.9.2 Quality control data shall be analyzed and, where they are found to be outside pre-defined criteria, planned actions shall be taken to correct the problem and to prevent incorrect results from being reported. QM-001 5.9.2 Correction and Prevention Policy and Details: As specified in QP-026

3. QP-026 Quality Control  Scope: * This procedure applies to all personnel within the laboratory * To ensure the accuracy and validity of test results  Definitions * Quality Control Sample (QCS): Matrix match; Known value * Control Chart: QCS data over time to show current results against acceptance criteria and trends of data over time.

4.  Mentor Lab(s)  Accrediting Body courses  Weekly lab meetings  Webinar (Control Chart and Trend Analysis by NY State Food Lab)  Quality Control Questionnaire  Individual one-on-one training Training

5. Quality Control Questionnaire

6. Overview of the MSCL Control Charts  Regulatory control charts Protein; Fat; Fiber; Dry Matter; Moisture; ADF; NDF; NIR protein, fat, fiber  Mercury and Inorganics control charts  Aflatoxin control charts  Total solids control chart  Residue control charts DEQ water, PAH and DOSS animal tissue  Petroleum products control charts

7. Mercury High Level Note: When two or more consecutive values fall outside 2 SD, it indicates it is time for recalibrating the instrument. Preliminary TestsDaily Tests 10.369710.3432 20.379520.3861 30.382830.4201 40.384140.4380 50.393850.4256 60.380760.4321 70.391570.4391 80.387280.4744 90.394290.4499 100.3859100.3998 110.3794110.3874 120.3843120.4436 130.3776130.4049 140.3904140.4100 150.3922150.3884 160.4125160.4204 170.3944170.3871 180.4078180.4141 190.4331190.3901 200.4134200.4273 STATISTICS210.4151 for Preliminary220.4180 tests230.4099 240.3948 Std Dev0.0149250.4099 Mean0.3917260.4186 UAL0.4366270.4129 UWL0.421628 LWL0.361829 LAL0.346930

8. Mercury Low Level Preliminary TestsDaily Tests 1 10.0058 2 20.0056 3 30.0060 4 40.0061 5 50.0062 6 60.0057 7 7 8 8 9 9 10 11 12 13 14 15 16 17 18 19 20 STATISTICS21 for Preliminary22 tests23 24 Std Dev0.0003625 Mean0.0059126 UAL0.0069927 UWL0.0066328 LWL0.0051929 LAL0.0048330 Note: Certified values were used to calculate the control limits.

9. Types of Data Plotted in Control Charts  Running a Quality Control Sample  Using Matrix Spikes  Proficiency Testing

10. Proficiency Testing Participation  AAFCO The Association of American Feed Control Officials  State Alflatoxin Share Program  AOAC International  FERN Food Emergency Response Network  Association of American Pesticide Control Officials Check Sample Program  Magruder  American Oil Chemists’ Society  National Forage Testing Association  ASTM International  Round Robin(s) with other State and Federal agencies  USDA FSIS  ERA

11. Control charts have improved the MSCL Quality Control  Control charts are monitored by the analyst entering data. “Out-of-control signals” on the control charts are investigated. * A single point outside 3 SD. * Two points outside 2 SD on the same side of the mean. * A run of eight points in a row are on the same side of the mean. * An increasing or decreasing trends  Initiate a corrective action according to the technical procedure.

12. Feedback from the Analyist I plot my QC standard with each sample set. The control chart is helpful in seeing the trends before I have a failure. I started plotting my instrument responses because it helps determine the need for maintenance or new commodities (columns, capillaries, standards or solvents Very helpful in determining steps to prevent inaccurate data. I plot the Standard Reference Material that is used for QC. Although, I still compare the measured results to the Certificate of Analysis in addition to the control chart. When reviewing sets of data the control charts are an easy reference to ensure the set of 10-20 samples has passing QC. By implementing control charts as a preventive measure fewer sample sets have to be repeated and there has been a decrease in the number of CARs related to PT failures.

13. If the Quality Manager ain’t happy nobody’s happy!!!

14. Crude Fiber Preliminary TestsDaily Tests 16.716.2 26.026.6 36.236.8 46.146.9 56.155.9 6 66.7 76.976.8 86.286.5 96.496.1 106.3106.2 117.0116.3 126.6127.0 136.7136.7 146.8147.0 156.9156.0 167.0166.9 176.9176.4 186.3186.3 196.0196.5 206.3206.7 STATISTICS216.5 for Preliminary226.6 tests236.4 246.0 Std Dev0.4256.9 Mean6.5266.3 UAL7.6276.3 UWL7.2286.2 LWL5.7296.0 LAL5.3306.1 Note: 20 data points were used to calculate the control limits.

15. Crude Fiber Continued Preliminary TestsDaily Tests 16.715.92 26.027.17 36.236.63 46.146.16 56.157.15 65.966.64 76.976.12 86.287.10 96.496.45 106.3106.56 117.0116.32 126.6126.73 136.7136.80 146.8146.82 156.9156.86 167.0166.87 176.9176.97 186.3186.09 196.0196.45 206.3207.23 STATISTICS216.51 for Preliminary227.02 tests235.92 24 Std Dev0.425 Mean6.526 UAL7.627 UWL7.228 LWL5.729 LAL5.330 Note: Use the same control limits as the previous control chart.

16. Aflatoxin Level 1 Preliminary TestsDaily Tests 1 113.5 2 213.6 3 312.4 4 415.1 5 515.5 6 67.7 7 712.3 8 812.9 9 911.8 10 10.2 11 12.1 12 10.6 13 8.8 14 14.0 15 11.6 16 17 18 19 20 STATISTICS21 for Preliminary22 tests23 24 Std Dev1.825 Mean12.126 UAL17.527 UWL15.728 LWL8.529 LAL6.730

17. Aflatoxin Level 2 Preliminary TestsDaily Tests 1 131.1 2 224.1 3 326.5 4 424.1 5 532.6 6 627.5 7 735.5 8 837.3 9 930.0 10 17.8 11 22.4 12 25.0 13 24.0 14 22.1 15 22.9 16 17 18 19 20 STATISTICS21 for Preliminary22 tests23 24 Std Dev4.725 Mean31.326 UAL45.427 UWL40.728 LWL21.929 LAL17.230

18. Total Solids Preliminary TestsDaily Tests 1 1122.5 2 2121.0 3 3126.5 4 4114.4 5 5119.2 6 6121.5 7 7124.1 8 8109.4 9 9122.9 10 120.4 11 134.4 12 115.8 13 119.4 14 114.9 15 125.8 16 121.2 17 122.3 18 19 20 STATISTICS21 for Preliminary22 tests23 24 Std Dev2.725 Mean120.026 UAL128.127 UWL125.428 LWL114.629 LAL111.930 Note: There are two data points out of 3 SD, but they are within acceptable limits.

19. Herbicide: Atrazine Percent of spike recovery Preliminary TestsDaily Tests TestB A 191180 2102289 382373 4764111 576564 6946123 7111772 8103896 9118972 101181081 1110511 129512 139913 1412414 1512415 169616 176217 186218 197019 208520 STATISTICS21 for Preliminary22 tests23 24 Std Dev19.225 Mean94.526 UAL152.127 UWL132.928 LWL56.129 LAL36.930 Note: Percent of spike recovery within 60 – 130%.

20. Anthracene Percent of spike recovery Preliminary TestsDaily Tests TestB A 190188 2 291 3101389 481487 592593 6886 792789 890893 991995 10901088 119411 129512 139413 149514 158715 169316 179117 189318 199119 208920 STATISTICS21 for Preliminary22 tests23 24 Std Dev4.025 Mean91.326 UAL103.327 UWL99.328 LWL83.329 LAL79.330 Note: Percent of spike recovery within 80 – 100%.