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Clean Water Act Analytical Methods

CWA Analytical Methods: Contaminants of Emerging Concern

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Pharmaceuticals and Personal Care Products (PPCPs) Methods Development

EPA has developed two analytical methods to identify and measure certain contaminants of emerging concern, specifically:
  • Method 1694 for a suite of 74 pharmaceuticals and personal care products
  • Method 1698 for a suite of 27 steroids and hormones, that may be determined in wastewater effluents and influents, and sewage sludge (biosolids)
These methods were validated in a single laboratory, and initially published in 2007. They have not undergone multi-laboratory validation, and have not been approved for NPDES compliance monitoring purposes at 40 CFR Part 136. Method 1694 is a compilation of at least four procedures with different extractions and analysis conditions. Since 2007, many laboratories have successfully implemented these methods or modified versions.

PPCP Methods; Not Approved Under Part 136

Number Method Title
1694 Pharmaceuticals and Personal Care Products in Water, Soil, Sediment, and Biosolids by HPLC/MS/MS (2007)
1698 Steroids and Hormones in Water, Soil, Sediment, and Biosolids by HRGC/HRMS (2007)

Contaminants of Emerging Concern in EPA Methods 1694 and 1698

Method 1694: 74 Pharmaceuticals and Personal Care Products in Water, Soil, Sediment, and Biosolids by HPLC/MS/MS
PPCP CAS # Classification
Acetaminophen 103-90-2 Antipyretic, analgesic
Albuterol 18559-94-9 Antiasthmatic
Ampicillin 69-53-4 β-lactam antibiotics
Anhydrochlortetracycline (ACTC) 13803-65-1 Chlorotetracycline degradate
Anhydrotetracycline (ATC) 4496-85-9 Chlorotetracycline degradate
Azithromycin 83905-01-5 Macrolide antibiotic
Caffeine 58-08-2 Stimulant
Carbadox 6804 07 05 Quinoxaline antibiotic
Carbamazepine 298-46-4 Anticonvulsant
Cefotaxime 63527-52-6 Cephalosporin antibiotic
Chlortetracycline (CTC) 57-62-5 Tetracycline antibiotic
Cimetidine 51481-61-9 Anti-acid reflux
Ciprofloxacin 85721-33-1 Quinoline antibiotic
Clarithromycin 81103-11-9 Macrolide antibiotic
Clinafloxacin 105956-97-6 Quinoline antibiotic
Cloxacillin 61-72-3 β-lactam antibiotics
Codeine 76-57-3 Opiate
Cotinine 486-56-6 Nicotine metabolite
Dehydronifedipine 67035-22-7 Nifedipine metabolite
Demeclocycline 127-33-3 Tetracycline antibiotic
Digoxigenin 1672-46-4 Immunohistochemical marker steroid
Digoxin 20830-75-5 Cardiac glycoside
Diltiazem 42399-41-7 Antihypertensive
1,7-Dimethylxanthine 611-59-6 Antispasmodic, caffeine metabolite
Diphenhydramine 58-73-1 Antihistamine
Doxycycline 564-25-0 Tetracycline antibiotic
Enrofloxacin 93106-60-6 Quinolone antibiotic
4-Epianhydrochlortetracycline (EACTC) 158018-53-2 Chlorotetracycline degradate
4-Epianhydrotetracycline (EATC) 4465-65-0 Chlorotetracycline degradate
4-Epichlortetracycline (ECTC) 14297-93-9 Chlorotetracycline degradate
4-Epioxytetracycline (EOTC) 14206-58-7 Oxytetracycline degradate
4-Epitetracycline (ETC) 23313-80-6 Tetracycline degradate
Erythromycin 114-07-8 Macrolide antibiotic
Erythromycin anhydrate 59319-72-1 Macrolide antibiotic
Flumequine 42835-25-6 Quinolone antibiotic
Fluoxetine 54910-89-3 SSRI antidepressant
Gemfibrozil 25812-30-0 Antilipemic
Ibuprofen 15687-27-1 Analgesic
Isochlortetracycline (ICTC) 514-53-4 Chlorotetracycline degradate
Lincomycin 154-21-2 Lincosamide antibiotic
Lomefloxacin 98079-51-7 Quinoline antibiotic
Metformin 657-24-9 Anti-diabetes drug
Miconazole 22916-47-8 Antifungal agent
Minocycline 10118-91-8 Tetracycline antibiotic
Naproxen 22204-53-1 Non-steroidal anti-inflammatory drug
Norfloxacin 70458-96-7 Quinoline antibiotic
Norgestimate 35189-28-7 Hormonal contraceptives
Ofloxacin 82419-36-1 Quinoline antibiotic
Ormetoprim 6981-18-6 Macrolide antibiotic
Oxacillin 66-79-5 β-lactam antibiotics
Oxolinic acid 14698-29-4 Quinolone antibiotic
Oxytetracycline (OTC) 79-57-2 Tetracycline antibiotic
Penicillin G 61-33-6 β-lactam antibiotics
Penicillin V 87-08-1 β-lactam antibiotics
Ranitidine 66357-35-5 Anti-acid reflux
Roxithromycin 80214-83-1 Macrolide antibiotic
Sarafloxacin 98105-99-8 Fluoroquinolone antibiotic
Sulfachloropyridazine 80-32-0 Sulfonamide antibiotic
Sulfadiazine 68-35-9 Sulfonamide antibiotic
Sulfadimethoxine 122-11-2 Sulfonamide antibiotic
Sulfamerazine 127-79-7 Sulfonamide antibiotic
Sulfamethazine 57-68-1 Sulfonamide antibiotic
Sulfamethizole 144-82-1 Sulfonamide antibiotic
Sulfamethoxazole 723-46-6 Sulfonamide antibiotic
Sulfanilamide 63-74-1 Sulfonamide antibiotic
Sulfathiazole 72-14-0 Sulfonamide antibiotic
Tetracycline (TC) 60-54-8 Tetracycline antibiotic
Thiabendazole 148-79-8 Fungicide and parasiticide
Triclocarban 101-20-2 Antimicrobial, disinfectant
Triclosan 3380-34-5 Antimicrobial, disinfectant
Trimethoprim 738-70-5 Pyrimidine antibiotic
Tylosin 1401-69-0 Macrolide antibiotic
Virginiamycin 11006-76-1 Macrolide antibiotic
Warfarin 81-81-2 Anticoagulant

Method 1698: 27 Steroids and Hormones in Water, Soil, Sediment, and Biosolids by HRGC/HRMS
Steroid/Hormone CAS # Classification
Androstenedione 63-05-8 anabolic agent
Androsterone 53-41-8 hormone metabolite
Equilenin 517-09-9 hormone replacement
Equilin 474-86-2 hormone replacement
17a-Ethynyl Estradiol (EE2) 57-63-6 ovulation inhibitor
Desogestrel 54024-22-5 ovulation inhibitor
Mestranol 72-33-3 ovulation inhibitor
Norethindrone 68-22-4 ovulation inhibitor
Norgestrel 6533-00-2 ovulation inhibitor
Campesterol 474-62-4 Phytosterol (plant sterol)
beta-Sitosterol 83-46-5 Phytosterol (plant sterol)
Stigmasterol 83-48-7 Phytosterol (plant sterol)
Beta-Stigmastanol 83-45-4 Phytosterol (plant sterol)
17a-Estradiol 57-91-0 Sex Hormone
17b-Estradiol (E2) 50-28-2 Sex Hormone
Estriol (E3) 50-27-1 Sex Hormone
Estrone (E1) 53-16-7 Sex Hormone
Progesterone 57-83-0 Sex Hormone
Testosterone 58-22-0 Sex Hormone
17a-Dihydroequilin 651-55-8 Sterol
Cholestanol 80-97-7 Sterol
Cholesterol 57-88-5 Sterol
Desmosterol 313-04-2 Sterol
Ergosterol 57-87-4 Sterol
b-Estradiol-3-benzoate 50-50-0 Sterol
Coprostanol 360-68-9 Sterol
Epi-Coprostanol 516-92-7 Sterol

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Other New Methods

EPA also has developed and single lab validated Method 1614A, a revised version of the high-resolution GC/MS procedure for the polybrominated diphenyl ethers (PBDEs) used as flame retardants and Method 1699, a new high-resolution GC/MS method for organochlorine pesticides.

Other Chemical Test Methods; Not Approved Under Part 136

Number Method Title
1614A Brominated Diphenyl Ethers in Water Soil, Sediment and Tissue by HRGC/HRMS (2010)
1699 Pesticides in Water, Soil, Sediment, Biosolids, and Tissue by HRGC/HRMS (2007)

These methods have been validated in a single laboratory and peer-reviewed. The PBDEs in Method 1614A are not currently regulated, and while many of the pesticides in Method 1699 are regulated, neither of these methods have been promulgated at 40 CFR Part 136.

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